A preparation method of polymaleic acid grafted cross-linked chitosan microspheres for heavy metal ion adsorption
A technology of chitosan microspheres and heavy metal ions, which is applied in the direction of alkali metal compounds, chemical instruments and methods, adsorption water/sewage treatment, etc., can solve the problems of failure to achieve adsorption effect and increase the cost of adsorbent preparation, and achieve control of preparation The effect of cost, good biocompatibility and non-toxicity, simple preparation method
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[0010] A method for preparing polymaleic acid grafted cross-linked chitosan microspheres for heavy metal ion adsorption, the specific method comprising the following steps: (1) making the 5 Da, chitosan with a deacetylation degree of 75%~97% is dissolved in 1%~2% (v / v) acetic acid or lactic acid aqueous solution to obtain a concentration of 1%~3% (w / v) chitosan Chitosan solution, the unit is g / mL; the chitosan solution is spray-dried at an inlet temperature of 180-220°C and an outlet temperature of 80-100°C to prepare chitosan microspheres; (2) Add chitosan microspheres into ethyl acetate, keep the temperature at 40-60°C, then add the cross-linking agent dropwise to the mixture, stir while adding, the stirring speed is 500-800 rpm; Continue to stir for 1-3 hours, collect the microspheres, wash with ethanol for 3-6 times, and dry in an oven at 30-70°C to obtain cross-linked chitosan microspheres; (3) cross-linked chitosan microspheres and FeCl 3 ·6H 2 O was added to distilled...
Embodiment 1
[0017] The viscosity average molecular weight is 4×10 5 Da, chitosan with a deacetylation degree of 90% is dissolved in acetic acid aqueous solution with a concentration of 2% (v / v) to obtain a chitosan solution with a concentration of 2.5% (w / v); set the inlet temperature to 220°C , the outlet temperature was 90°C, and the chitosan solution was spray-dried to prepare chitosan microspheres; the prepared chitosan microspheres were added to ethyl acetate, and the mixture of chitosan microspheres and ethyl acetate was The ratio was 2.5:100 (g:mL), and the temperature was maintained at 50°C. Then, glutaraldehyde was added dropwise to the mixture, and stirred while adding, at a stirring speed of 600 rpm, until the final concentration of glutaraldehyde in the system was reach 1%; continue to stir for 1 h after the dropwise addition, collect the microspheres, wash with ethanol three times, and dry in a 50°C oven to obtain cross-linked chitosan microspheres; cross-linked chitosan mic...
Embodiment 2
[0019] The viscosity average molecular weight is 3×10 5Da, chitosan with a degree of deacetylation of 75% is dissolved in an aqueous solution of acetic acid with a concentration of 1.5% (v / v) to obtain a chitosan solution with a concentration of 1% (w / v); set the inlet temperature to 200°C , the outlet temperature was 80°C, and the chitosan solution was spray-dried to prepare chitosan microspheres; the prepared chitosan microspheres were added to ethyl acetate, and the mixture of chitosan microspheres and ethyl acetate was The ratio was 4:100 (g:mL), and the temperature was maintained at 40°C. Then, benzaldehyde was added dropwise to the mixture, and stirred while adding, at a stirring speed of 800 rpm, until the final concentration of benzaldehyde in the system reached 2 %,; continue to stir for 2 h after the dropwise addition, collect the microspheres, wash with ethanol for 6 times, and dry in an oven at 60°C to obtain cross-linked chitosan microspheres; cross-linked chitosa...
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