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Surface imprinting chitosan microspheres for efficiently selecting heavy-metal ions and preparation method for surface imprinting chitosan microspheres

A technology of chitosan microspheres and heavy metal ions, applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of complex synthesis operations and harsh conditions, and achieve simple synthesis operations , Mild cross-linking conditions and wide range of sources

Active Publication Date: 2016-01-06
南京华创环境技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the complicated synthetic operation and harsh conditions of existing surface imprinted adsorbents, the need for many highly toxic auxiliary agents, and neglecting the secondary assembly of pre-assembled complexes of functional monomers and template ions on the surface of activated substrates, the present invention provides a Surface-imprinted chitosan microspheres for efficient selection of heavy metal ions and their preparation method, based on a simple and novel adsorption-post-crosslinking method to prepare surface ion-imprinted chitosan microspheres, the new adsorbent has ultra-high heavy metal ion recognition and Separation ability

Method used

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  • Surface imprinting chitosan microspheres for efficiently selecting heavy-metal ions and preparation method for surface imprinting chitosan microspheres
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  • Surface imprinting chitosan microspheres for efficiently selecting heavy-metal ions and preparation method for surface imprinting chitosan microspheres

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Embodiment 1

[0034] A kind of surface imprinted chitosan microsphere of ultrahigh selective separation Cu (II), its step is:

[0035] (1) Preparation of chitosan microspheres: accurately weigh 4g chitosan powder and dissolve in 100mL volume concentration of 2% acetic acid solution, then drip the chitosan solution into a 250mL coagulation bath with a peristaltic pump and solidify into a ball , the coagulation bath is prepared by 200mL distilled water, 16g sodium hydroxide and 50mL ethanol, after standing for 30min, chitosan microspheres (referred to as CS) are filtered out, washed and placed in distilled water for preservation;

[0036] (2) Preparation of carboxylated chitosan microspheres: Weigh the chitosan microspheres gained in step (1) and place 100 mL of mass concentration in 8% sodium chloroacetate aqueous solution, adjust pH=13 with NaOH, at 80° C. Heated and stirred in an oil bath for 10 hours to obtain chloromethylated chitosan microspheres (referred to as CS-COONa), took out the ...

Embodiment 2

[0047] With embodiment 1, difference is:

[0048] The volume fraction of acetic acid is 8% in the step (1), and the mass fraction of chitosan solution is 2%, and coagulation bath is prepared by 200mL distilled water, 8g sodium hydroxide and 10mL ethanol;

[0049] The mass concentration of sodium chloroacetate in step (2) is 2%, adjust pH=8 with alkaline solution, heat to 60°C and stir for 5h;

[0050] In step (3), the molecular weight of polyethyleneimine is 7500, and the molar ratio of polyethyleneimine to heavy metal ions is 4:1. After adding copper nitrate solution (concentration is 20mmol / L) and shaking for 10h, add chloromethylation Chitosan microspheres (dosing amount is 50g / L) are shaken and adsorbed at 60°C for 60h; Cross-linking reaction at 80℃ for 10h;

[0051] The mass concentration of the EDTA solution in the step (4) is 20%, and the alkali solution is a 1 mmol / L NaOH solution.

[0052] Gained microspheres have an adsorption capacity of 0.61mmol / g under the same...

Embodiment 3

[0054] With embodiment 1, difference is:

[0055] The volume fraction of acetic acid is 6% in the step (1), and the mass fraction of chitosan solution is 3%, and coagulation bath is prepared by 200mL distilled water, 32g sodium hydroxide and 80mL ethanol;

[0056] The mass concentration of sodium chloroacetate in step (2) is 20%, adjust pH=14 with alkaline solution, heat to 20°C and stir for 8h;

[0057] In step (3), the molecular weight of polyethyleneimine is 9000, and the molar ratio of polyethyleneimine to heavy metal ion is 3:1. After adding copper nitrate solution (concentration is 1mmol / L) and shaking for 8h, add chloromethylation Chitosan microspheres (dosing amount is 20g / L) are shaken and adsorbed at 40°C for 10h; Cross-linking reaction at 20°C for 3 hours;

[0058] The mass concentration of the EDTA solution in the step (4) is 4%, and the alkali solution is a 0.5 mmol / L NaOH solution.

[0059] Gained microspheres have an adsorption capacity of 0.84mmol / g under th...

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Abstract

The invention discloses surface imprinting chitosan microspheres for efficiently selecting heavy-metal ions and a preparation method for the surface imprinting chitosan microspheres and belongs to the field of adsorbent synthesis. The preparation method comprises the steps of carrying out carboxylation modification on chitosan by adopting sodium chloroacetate so as to obtain electronegative carboxylated chitosan microspheres, then, carrying out surface adsorption by using a pre-assembled complex of polyethyleneimine and the heavy-metal ions, then, fixing imprinted sites by using epoxy chloropropane as a cross-linking agent, finally, eluting the heavy-metal ions by adopting an ethylenediamine tetraacetic acid solution, and carrying out freeze-drying, thereby obtaining the surface imprinting chitosan microspheres. The surface imprinting chitosan microspheres are simple in synthesis process, low in preparing cost and stable in surface imprinting hole spatial-configuration, thereby having a specific recognition function on template heavy-metal ions, and the high-selectively separated removal and resource recovery of the heavy-metal ions from wastewater can be realized, so that environmental and economic benefits are remarkable.

Description

technical field [0001] The invention belongs to the field of adsorbent synthesis, and more specifically relates to a surface imprinted chitosan microsphere for efficiently selecting heavy metal ions and a preparation method thereof. Background technique [0002] The high concentration of inorganic salts coexisting with heavy metal ions in industrial wastewater will seriously weaken the removal efficiency of adsorbents for target ions due to the site competition effect. How to selectively separate and recover heavy metal ions from high-salt wastewater has important environmental and economic significance. At the same time, there is an urgent need for functional materials with high-efficiency separation performance. Chelating adsorbents can achieve selective adsorption and separation of target ions by utilizing the difference in affinity between the coordination functional groups fixed on the substrate and heavy metal ions. However, most of the current research focuses on opt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30C02F1/28C02F1/62
Inventor 刘福强朱长青朱增银张艳红韦蒙蒙张小朋凌晨李爱民
Owner 南京华创环境技术研究院有限公司
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