Low-molecular-weight C6-carboxyl chitin and preparation method thereof
A low-molecular-weight, chitin technology, applied in the field of biopolymer chemistry, can solve the problems of destroying the original structure of chitin, high degree of deacetylation, and low degree of reaction completeness, and achieves favorable biocompatibility and low degree of deacetylation. , the effect of short process flow
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[0021] As an example, the preparation method of C6-carboxychitin provided by the invention comprises the following steps:
[0022] (1) Use a functional solvent to prepare a homogeneous solution from the pulverized raw material chitin to realize the transformation of the compact structure of chitin to a loose structure, the dissolution of biopolymers, and the depolymerization of high molecular weight to low molecular weight. Contains one or more of phosphoric acid, sulfuric acid and hydrochloric acid;
[0023] (2) directly adding an acidic medium oxidizing agent and a catalyst to the solution obtained in step (1) to carry out an oxidation reaction so that the C6 hydroxyl group is oxidized to a carboxyl group, and further depolymerizes chitin;
[0024] (3) adjusting the pH of the reaction solution obtained in step (2) to 5 to 6 to obtain a crude product or a refined product through refining.
[0025] Preferably, the amount of functional solvent used in step (1) is 2 to 4 times ...
Embodiment 1
[0037]The flaky chitin from snow crab was processed into 0.25mm pieces with a pulverizer and set aside. Mix phosphoric acid solution with a mass concentration of 85% and hydrochloric acid solution with a mass concentration of 33% at a volume ratio of 10:11 to prepare a functional solvent for later use. The oxidizing agent consists of sodium nitrate. The catalyst is sodium nitrite. Take 60 grams of chitin fragments and add them to a 500mL three-neck flask, add 145 grams of functional solvent, heat to 85°C, and keep warm for 30 minutes. When the chitin is completely dissolved and the solution is homogeneous, stop heating and naturally cool to 60°C. First put in half of the oxidant and catalyst, and when the catalytic reaction reaches equilibrium, add the other half of the oxidant and catalyst. A total of 34 grams of sodium nitrate and 7 grams of sodium nitrite were added. The initial temperature is controlled at 60°C, and then the reaction temperature is slowly increased, whi...
Embodiment 2
[0039] The irregular massive chitin from crayfish is processed to 0.15mm fragments with a pulverizer and set aside. Phosphoric acid with a mass concentration of 85%, sulfuric acid with a mass concentration of 61% and hydrochloric acid with a mass concentration of 33% are mixed according to a volume ratio of 20:20:33 to prepare a functional solvent for future use. The oxidizing agent consists of sodium nitrate. The catalyst is sodium nitrite. Take 80 grams of chitin fragments and add them to a 500 mL three-neck flask, add 210 grams of functional solvent, heat to 80°C, keep warm for 30 minutes, the chitin is completely dissolved, and cool down to 65°C. The oxidizer and half of the catalyst were put in, and the other half of the catalyst was added after 1.5 hours. A total of 45 grams of sodium nitrate and 8 grams of sodium nitrite were added. The oxidation reaction time is 4-5 hours in total, and the pH of the reaction solution is adjusted to 6 with sodium carbonate. Remove u...
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