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Method for preparing hydroxypropylated chitosan ferrous derivate by magnetic field reinforcement

A technology of ferrous hydroxypropyl chitosan and magnetic field enhancement is applied in the field of preparation of chitosan derivatives, which can solve the problems of long reaction time, low derivatization efficiency, large amount of reactants, etc. The effect of shortening the reaction time and improving the reaction efficiency

Inactive Publication Date: 2011-12-28
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using traditional derivatization methods, the reaction time is long, the amount of reactants is large, and the derivatization efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) 1g chitosan (average molecular weight 50000Da, degree of deacetylation 93.6%) was dissolved in 100ml of acetic acid solution (pH 1.0) with a weight fraction of 2%, and swelled for 2h, then diluted with absolute ethanol to prepare 5mg / ml chitosan solution.

[0023] (2) Slowly add ferrous ammonium sulfate solution with a concentration of 2 mol / L so that the weight ratio of chitosan to ferrous ammonium sulfate is 1:4. The above reaction system was placed under a magnetic field of 60 mT, stirred and refluxed at 50° C. for 0.5 h, and the pH of the solution was adjusted to 2.0. Separation by filtration, precipitation is chitosan ferrous complex.

[0024] (3) Using propylene oxide and the obtained product in a weight ratio of 15:1, under the action of a magnetic field of 60 mT, reflux at a constant temperature of 70° C. for 3 hours. Filter, then wash the precipitate with absolute ethanol, and vacuum-dry it at constant temperature (temperature 60°C) for 1 hour to obtain ...

Embodiment 2

[0026] (1) 1g chitosan (average molecular weight 40000Da, degree of deacetylation 93.6%) was dissolved in 100ml of 3% acetic acid solution (pH 1.5) by weight fraction, swelled for 2.5h, and then diluted with absolute ethanol to prepare 4mg / ml chitosan solution.

[0027] (2) Slowly add ferrous ammonium sulfate solution with concentration of 1.8mol / L dropwise, so that chitosan: ferrous ammonium sulfate (weight ratio)=1:5. The above reaction system was placed under a magnetic field of 80 mT, stirred and refluxed at 50° C. for 3 h, and the pH value of the solution was adjusted to 3.0. Separation by filtration, precipitation is chitosan ferrous complex.

[0028] (3) Using propylene oxide and the obtained product in a weight ratio of 18:1, under a magnetic field of 80 mT, reflux at a constant temperature of 60° C. for 5 hours. Filter, wash the precipitate with absolute ethanol, and vacuum-dry at constant temperature (temperature 60° C.) for 1.2 h to obtain 99.9% pure product of h...

Embodiment 3

[0030] (1) Dissolve 1g of chitosan (average molecular weight 30000Da, degree of deacetylation 93.6%) in 100ml of 4% acetic acid solution (pH 2) by weight fraction, swell for 3h, add absolute ethanol to dilute, and prepare 3mg / ml Chitosan solution.

[0031] (2) Slowly add ferrous ammonium sulfate solution with a concentration of 1.6 mol / L so that the weight ratio of chitosan to ferrous ammonium sulfate is 1:6. The above reaction system was placed under a magnetic field of 100 mT, stirred and refluxed at a temperature of 50° C. for 4 hours, and the pH value of the solution was adjusted to 4.0. Separation by filtration, precipitation is chitosan ferrous complex.

[0032] (3) Using propylene oxide and the obtained product in a weight ratio of 20:1, under the action of a magnetic field of 100 mT, reflux reaction at a constant temperature of 65° C. for 7 hours. After separation by filtration, the precipitate was washed with absolute ethanol, and vacuum-dried at constant temperatur...

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Abstract

The invention discloses a method for preparing hydroxypropylated chitosan ferrous derivant by magnetic field reinforcement. Chitosan is dissolved in acetum with pH of 1.0-3.5, chitosan and ammonium ferrous sulphate are prepared into solution by weight ratio of 1:4-8, reaction is carried out in the magnetic field with intensity of 60-150mT, and separation is carried out, thus obtaining chitosan ferrous complex. Epoxypropane is added by the weight ratio of the chitosan ferrous complex and epoxypropane to be 1:10-25, stirring is carried out at the constant temperature of 60-70 DEG C in the magnetic field, and reflux reaction is carried out for 3-10h. Filtering is carried out, absolute alcohol is used for washing, and vacuum drying at constant temperature is carried out, thus obtaining hydroxypropylated chitosan ferrous complex product. The method for preparing chitosan derivate by magnetic field reinforcement provided by the invention can improve reaction efficiency of chitosan derivatization and can prepare chitosan derivate with excellent absorption and flocculation properties.

Description

technical field [0001] The invention relates to a preparation method of chitosan derivatives, in particular to a method for preparing ferrous hydroxypropyl chitosan derivatives by strengthening a magnetic field. Background technique [0002] Chitin, also known as chitin and chitin, is a natural polymer polysaccharide. It is widely distributed in the shells of crustaceans, shrimps and crabs in nature, the shells of insects and the cell walls of some fungi. The annual biosynthesis amount reaches 1×10 11 tons, the output is second only to cellulose, and it is the second largest natural renewable resource on earth. Chitosan (CS for short), also known as chitosan or chitosan, is the deacetylation product of chitin. In 1977, the Japanese used chitosan as a natural flocculant to treat wastewater for the first time. In the same year, the first international conference on chitin / chitosan was held in Boston, USA. Chitosan has good adsorption, moisture retention, wettability, film-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
Inventor 郭祀远叶盛权王兆梅郑必胜肖凯军杨晋青
Owner SOUTH CHINA UNIV OF TECH
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