Polyoxyethylene polyoxypropylene-chitosan block copolymer, bone hemostatic material and preparation method thereof
A polyoxyethylene polyoxypropylene, block copolymer technology, applied in the field of medicine, can solve the problems of long-term retention of foreign matter in the body, prone to infection and pain, and inability to be absorbed by the body, so as to increase the molecular weight and high product quality rate , Improve the effect of biocompatibility
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[0048] According to a first aspect of the present invention, a kind of preparation method of polyoxyethylene polyoxypropylene-chitosan block copolymer is provided, comprising the steps:
[0049] (a) react polyoxyethylene polyoxypropylene block copolymer and activator in solvent, precipitate, solid-liquid separation, obtain activated polyoxyethylene polyoxypropylene block copolymer;
[0050] (b) Chitosan and the activated polyoxyethylene polyoxypropylene block copolymer obtained in step (a) carry out graft copolymerization reaction in acid solution, precipitate, and separate solid and liquid to obtain polyoxyethylene polyoxypropylene-shell Polysaccharide block copolymers;
[0051] Wherein, the activator includes N,N'-carbonyldiimidazole.
[0052] The present invention adopts a two-step method to synthesize polyoxyethylene polyoxypropylene-chitosan block copolymer, and first utilizes N,N'-carbonyldiimidazole to activate the polyoxyethylene polyoxypropylene block copolymer conta...
Embodiment 1
[0099] A kind of preparation method of polyoxyethylene polyoxypropylene-chitosan block copolymer, comprises the steps:
[0100] (1) Synthetic activated polyoxyethylene polyoxypropylene block copolymer:
[0101] Dissolve 30g of polyoxyethylene polyoxypropylene block copolymer, 5.89g of N,N'-carbonyldiimidazole in 150ml of 1,4-dioxane and dimethyl sulfoxide with a volume ratio of 2:1 In the reagent, the reaction was stirred for 12 h at a temperature of 37 °C. After the reaction, stir under ice-bath conditions and add anhydrous ether dropwise, filter to obtain a precipitate, wash three times with anhydrous ether, and vacuum-dry to obtain an activated polyoxyethylene polyoxypropylene block copolymer as a white precipitate.
[0102] (2) Synthetic polyoxyethylene polyoxypropylene-chitosan block copolymer:
[0103] Dissolve 4g of chitosan and 8g of activated polyoxyethylene polyoxypropylene block copolymer in 0.1mol / L hydrochloric acid solution, stir for 12h at a temperature of 37°...
Embodiment 2
[0107] A kind of preparation method of polyoxyethylene polyoxypropylene-chitosan block copolymer, comprises the steps:
[0108] (1) Synthetic activated polyoxyethylene polyoxypropylene block copolymer:
[0109] Dissolve 50g of polyoxyethylene polyoxypropylene block copolymer and 9.75g of N,N'-carbonyldiimidazole in 200ml of 1,4-dioxane and dimethyl sulfoxide mixed reagent with a volume ratio of 2:1 , the reaction was stirred at a temperature of 37° C. for 12 h. After the reaction, stir under ice-bath conditions and add anhydrous ether dropwise, filter to obtain a precipitate, wash three times with anhydrous ether, and vacuum-dry to obtain an activated polyoxyethylene polyoxypropylene block copolymer as a white precipitate.
[0110] (2) Synthetic polyoxyethylene polyoxypropylene-chitosan block copolymer:
[0111] Dissolve 6g of chitosan and 8g of activated polyoxyethylene-polyoxypropylene block copolymer in 0.1mol / L hydrochloric acid solution, stir for 12h at a temperature of...
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