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

Active Publication Date: 2019-07-16
OCEAN UNIV OF CHINA +1
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  • Summary
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Problems solved by technology

In recent years, research has focused on grafting chitosan with functional groups and then preparing microspheres and cross-linking, which has increased the stability and adsorption performance of the product to a certain extent, but there are still certain defects: (1) grafting Part of the functional groups of the branches are still involved in the cross-linking; (2) only part of the functional groups are exposed on the surface of the microspheres to play an adsorption role; (3) while increasing the cost of the preparation of the adsorbent, the ideal adsorption effect is not achieved

Method used

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preparation example Construction

[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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Abstract

The invention relates to a preparation method of polymaleic acid grafting and crosslinking chitosan micro-spheres for heavy metal ion adsorption, and belongs to the field of water environment protection. The method includes the steps: preparing the chitosan micro-spheres by a spray drying method, and performing crosslinking for the chitosan micro-spheres to prepare the crosslinking chitosan micro-spheres; separating and drying the crosslinking chitosan micro-spheres, grafting maleic acid to the surfaces of the crosslinking chitosan micro-spheres in a homopolymer manner under the condition of N2 protection, and separating, washing and drying mixture to obtain the polymaleic acid grafting and crosslinking chitosan micro-spheres. The preparation method is simple, stable in process, the chitosan micro-spheres are crosslinked, the stability and the mechanical performance of the chitosan micro-spheres in acid solution are improved, H2O2-Fe3+ serves as initiating agents, the maleic acid is furthest grafted onto C2-NH2, C6-CH2OH and C3-OH of chitosan molecules in a homopolymer manner, the adsorption capacity of the micro-spheres is effectively improved, and preparation cost is controlled. The prepared polymaleic acid grafting and crosslinking chitosan micro-spheres are round in shape, uniform in particle diameter, safe to use and convenient to store and transport, has efficient adsorption performance for heavy metal ions and can be widely used for the field of water environment protection. The preparation method has high economical exploitation potentiality.

Description

technical field [0001] The invention belongs to the field of water environment protection and relates to a method for preparing polymaleic acid grafted cross-linked chitosan microspheres for heavy metal ion adsorption. Background technique [0002] Heavy metal ions with high toxicity and non-degradability have brought serious harm to the natural environment and human health. Therefore, the search for effective materials and methods to control heavy metal pollution has attracted worldwide attention. At present, the methods for removing heavy metals in water environment mainly include adsorption, chemical precipitation, membrane filtration, ion exchange, reverse osmosis, electrodialysis, flocculation and so on. Among them, the adsorption method is widely used because of its simple operation, high efficiency, low cost, good reusability, and no secondary pollution. Chemisorption is one of the main forms of adsorption, which mainly uses specific functional groups to bind heavy m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F101/20
CPCB01J20/267B01J20/28019B01J2220/4812C02F1/285C02F2101/20
Inventor 刘成圣党奇峰于真真张伯年高辉
Owner OCEAN UNIV OF CHINA
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