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A technology of chitosan and phosphorylation, which is applied in the field of biochemical industry to achieve the effects of high yield, simple and easy operation, and high degree of substitution
Inactive Publication Date: 2013-07-31
WUHAN INSTITUTE OF TECHNOLOGY
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At present, there are few studies on phosphorus derivatives of chitosan, but its potential application fields involve many aspects, such as metal chelation, biomedicine, drug carrier, tissue engineering materials for bone repair, bacteriostats and fuel cells, etc.
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Embodiment 1
[0020] Mix 2g of chitosan and 14ml of methanesulfonic acid evenly, then add 6g of phosphorus pentoxide, under the protection of nitrogen, keep mechanical stirring at 2°C for 2 hours; add 70ml of ether to the obtained reaction system for precipitation, centrifuge . Then wash the precipitate with 42ml acetone and 42ml methanol successively. The precipitate was then dissolved with 50 ml of deionized water. The turbid liquid was dialyzed with a molecular weight cut-off of 6000, then concentrated in vacuum, and the concentrated liquid was freeze-dried to obtain the product.
[0021] figure 1 Be the infrared spectrum contrast figure of chitosan and embodiment 1 gained phosphorylated chitosan, wherein figure 1 (a) is the infrared spectrogram of chitosan, figure 1 (b) is the infrared spectrogram of embodiment 1 gained phosphorylated chitosan. For chitosan, 3500-3400cm -1 It is the stretching vibration absorption band of hydroxyl OH; 2878cm -1 is the methine CH on the sugar ring...
Embodiment 2
[0033] Mix 3g of chitosan and 21ml of methanesulfonic acid evenly, then add 8g of phosphorus pentoxide, under the protection of nitrogen, keep mechanically stirring at 4°C, then slowly add 2g of phosphorus pentoxide, and react for 3 hours; Add 100 ml of diethyl ether to the resulting reaction system for precipitation and centrifugation. Then wash with 60ml acetone and 60ml methanol successively. Then dissolve the precipitate with 80ml deionized water. The turbid liquid was dialyzed with a molecular weight cut-off of 3500, then concentrated in vacuum, and the concentrated liquid was freeze-dried to obtain the product.
[0034] After testing, the degree of substitution of the obtained phosphorylated chitosan was 1.27.
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Abstract
The present invention relates to a chitosan phosphorylation modification method, which comprises the following steps: 1) a reaction, wherein under a condition of a temperature of 0-5 DEG C, 1 g of chitosan is dissolved into 7 ml of methyl sulfonic acid, 0.5-3.5 g of phosphorus pentoxide is added, and a continuous mechanical stirring reaction is performed for 2-3 h in the protection of nitrogen gas; and 2) separation, wherein ether is added to the reaction system obtained from the step 1) to carry out precipitation, centrifugation is performed, acetone and methanol are sequentially adopted to wash the precipitate, deionized water is adopted to dissolve the precipitate, the turbid solution is sequentially subjected to dialysis and vacuum concentration, and the concentrated solution is subjected to freeze-drying to obtain the product. The chitosan phosphorylation modification method has the following advantages that: 1, the method has characteristics of simpleness, easy operation, high yield, and environmental protection, and is suitable for industrial production in reactions; 2, the obtained product has a high substitution degree, and the phosphate has strong chelating ability; and 3, the obtained product can be widely used in agriculture, textile, medicine, food, cosmetics, environmental protection and other fields.
Description
technical field [0001] The invention belongs to the field of biochemical industry, and in particular relates to a method for phosphorylation modification of chitosan. Background technique [0002] Chitin is also called chitin, its chemical name is (1,4)-2-acetylamino-2-deoxy-β-D-glucan, and its molecular weight is several million. The structure of chitin is very similar to that of cellulose. just C for each residue 2 The upper hydroxyl group is replaced by an acetylated amino group. Chitin is difficult to dissolve in common solvents due to the hydrogen bond between molecules and molecules, which greatly limits the further application of chitin. In order to increase its water solubility, chitosan is usually prepared by deacetylating chitin. Chitosan can only be dissolved under acidic conditions, which limits its application range. [0003] Chemical modification of chitosan is one of the means to improve its basic properties and expand its application fields. The modifie...
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