A kind of preparation method of chitosan oligosaccharide
A technology of chitosan oligosaccharides and reaction bottles, which is applied in the preparation of sugar derivatives, chemical instruments and methods, amino sugars, etc., can solve the problems of long reaction cycle, high cost of enzymatic degradation, environmental pollution by strong acid solvents, etc., and achieve finished products The effect of good purity, low cost and easy control conditions
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Embodiment 1
[0013] Add 10g of ionic liquid 1-ethyl-3-methylimidazole acetate (EMimAC) into the reaction flask, put the reaction flask into an oil bath to control the temperature at 100°C, then add 1.0g of chitin to the reaction flask, and magnetically Under stirring, the chitin was completely dissolved until the solution was transparent; then, 1.5 g of acidic ionic liquid 1-sulfopropylpyridinium bisulfate was added to the reaction flask, and the temperature of the oil bath was raised to 150°C for reaction, and divided into Add hydrogen peroxide with a mass fraction of 30% to the reaction bottle in batches, add 0.2ml each time, add once every 2h, stop the reaction after 12h; cool the reaction system to room temperature with deionized water, and centrifuge the solution in the reaction bottle Remove the insolubles, add 3 times the volume of ethanol to the centrifuged filtrate to precipitate chitooligosaccharides, then centrifuge, wash, and freeze-dry to obtain chitooligosaccharides with a yie...
Embodiment 2
[0015] Add 10g of ionic liquid 1-butyl-3-methylimidazolium chloride (BMimCl) to the reaction flask, put the reaction flask into an oil bath to control the temperature at 100°C, then add 1.5g of chitin to the reaction flask, and stir it magnetically Dissolve chitin completely until the solution is transparent; then add 0.5g of acidic ionic liquid 1-sulfopropylpyridinium bisulfate to the reaction flask, control the temperature at 60°C for reaction, and add to the reaction flask in batches Add hydrogen peroxide with a mass fraction of 30%, add 0.2ml each time, add once every 2h, and stop the reaction after 12h; cool the reaction system to room temperature with deionized water, centrifuge the solution in the reaction bottle to remove insoluble matter, and pour it into the filtrate Add 3 times the volume of ethanol to precipitate chitosan oligosaccharides, and then centrifuge, wash, and freeze-dry to obtain chitosan oligosaccharides with a yield of 45%; the discarded filtrate can be...
Embodiment 3
[0017] Add 10g of ionic liquid 1-allyl-3 methylimidazolium chloride (AMimCl) to the reaction flask, put the reaction flask into an oil bath to control the temperature at 100°C, then add 0.3g of chitin to the reaction flask, and stir it magnetically Dissolve chitin completely until the solution is transparent; then add 0.5g of acidic ionic liquid 1-sulfopropylpyridinium bisulfate to the reaction flask, control the temperature at 100°C for reaction, and add to the reaction flask in batches Add hydrogen peroxide with a mass fraction of 30%, add 0.2ml each time, add once every 2h, and stop the reaction after 12h; cool the reaction system to room temperature with deionized water, and centrifuge the solution in the reaction bottle to remove insoluble matter. Add 3 times the volume of ethanol to the filtrate to precipitate chitooligosaccharides, and then centrifuge, wash, and freeze-dry to obtain chitooligosaccharides with a yield of 59%; the discarded filtrate can be recycled by rota...
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