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Amino-protected crosslinking magnetic chitosan composite adsorbent and preparation method thereof

A composite adsorption and chitosan technology, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., to achieve the effect of simple preparation process, fast adsorption rate and good reusability

Inactive Publication Date: 2012-10-24
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention prepares the cross-linked magnetic chitosan composite adsorbent of amino protection, and chitosan, magnetic Fe3O 4 or γ-Fe2O3, inorganic materials, and polymer compounds are combined to obtain high amino content, high adsorption capacity, and fast adsorption rate , and can be recovered by the action of an external magnetic field, the adsorbent with good reusability, similar research has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Dissolve 2g chitosan in 100mL 2% (V / V) acetic acid aqueous solution, weigh 1g γ-Fe 2 o 3 , add 50ml of water, sonicate for 10min to disperse evenly, take 1g of polyvinyl alcohol to dissolve (80°C), mix the two solutions, and stir for 2h. Add 150mL toluene and 1.5mL emulsifier (Span80), and continue to stir for 1h to make the system uniform. Add 30mL formaldehyde, cross-linking reaction 2h. After the reaction, the mixture is poured into a solution (V 乙醇 :V 氢氧化钠溶液 =1:1). After stirring, it was filtered with suction and washed repeatedly with ether, ethanol and water. Put the obtained microspheres into 300 mL of epichlorohydrin with a concentration of 0.06 mol / L, adjust the pH to 10, and react in a water bath at 50°C-60°C for 4 hours. Filter and wash with water until neutral. The product was placed in 200ml of 0.5mol / L HCl, stirred overnight to remove the Schiff base, filtered, the microspheres were neutralized with 0.1mol / L NaOH solution, washed with water until ne...

Embodiment 2

[0038] Dissolve 2g chitosan in 100mL 2% (V / V) acetic acid aqueous solution, weigh 1g γ-Fe 2 o 3 , add 50ml of water, sonicate for 10min to disperse evenly, dissolve 1g of gelatin (50°C), mix the two solutions, and stir for 2h. Add 150mL liquid paraffin, 1.5mL emulsifier (Span80), and continue stirring for 1h to make the system uniform. Add 30mL formaldehyde, cross-linking reaction 2h. After the reaction, the mixture was poured into the solution of 1000ml absolute ethanol and sodium hydroxide (mass fraction 10%) (V 乙醇 :V 氢氧化钠溶液 =1:1). After stirring, it was filtered with suction and washed repeatedly with ether, ethanol and water. Put the obtained microspheres into 300 mL of epichlorohydrin with a concentration of 0.06 mol / L, adjust the pH to 10, and react in a water bath at 50°C-60°C for 4 hours. Filter and wash with water until neutral. The product was placed in 200ml of 0.5mol / L HCl, stirred overnight to remove the Schiff base, filtered, the microspheres were neutrali...

Embodiment 3

[0041] Dissolve 2g chitosan in 100mL 2% (V / V) acetic acid aqueous solution, weigh 1g γ-Fe 2 o 3 , add 50ml of water, sonicate for 10min to disperse evenly, take 1g of polyethyleneimine to dissolve, mix the two solutions, and stir for 2h. Add 150mL toluene and 1.5mL emulsifier (Span80), and continue to stir for 1h to make the system uniform. Add 30mL formaldehyde, cross-linking reaction 2h. After the reaction, the mixture is poured into the solution of 800ml dehydrated alcohol and sodium hydroxide (mass fraction 10%) (V 乙醇 :V 氢氧化钠溶液 =1:1). After stirring, it was filtered with suction and washed repeatedly with ether, ethanol and water. Put the obtained microspheres into 300 mL of epichlorohydrin with a concentration of 0.06 mol / L, adjust the pH to 10, and react in a water bath at 50°C-60°C for 4 hours. Filter and wash with water until neutral. The product was placed in 200ml of 0.5mol / L HCl, stirred overnight to remove the Schiff base, filtered, the microspheres were neutr...

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Abstract

The invention relates to an amino-protected crosslinking magnetic chitosan composite adsorbent and a preparation method of the amino-protected crosslinking magnetic chitosan composite adsorbent. The preparation method comprises the following steps: enabling formaldehyde and amino on the chitosan to react to generate Schiff's base protected amino; crosslinking by using epichlorohydrin; and finally, carrying out acidolysis to remove the Schiff's base to recover the amino to obtain the amino-protected crosslinking magnetic chitosan composite adsorbent. The amino-protected crosslinking magnetic chitosan composite adsorbent comprises a magnetic chitosan and probably comprises a high molecular compound and / or an inorganic material. The amino-protected crosslinking magnetic chitosan composite adsorbent has the characteristics that the preparation process of the composite adsorbent is simpler, and the process parameters are easy to control; the adsorption capacity and the adsorption speed of the composite adsorbent are large and high, and the composite adsorbent can be recovered through an external magnetic field, so the reusability of the composite adsorbent is good. The composite adsorbent can be hopefully used for treating waste water containing heavy metal ions, protein and dye.

Description

[0001] technical field [0002] The invention relates to an amino-protected cross-linked magnetic chitosan composite adsorbent and a preparation method thereof. Background technique [0003] Chitosan (CS) is the deacetylation product of chitin, the second largest biomass resource in nature, with abundant sources. Chitosan has good biocompatibility and degradability. The abundant hydroxyl and amino groups on its molecular chain make it have good affinity for metal ions, dyes, proteins and other substances. It is widely used as an adsorbent for dyes, Treatment of water bodies such as heavy metal ions and natural organic matter. [0004] The abundant amino groups on the molecular chain of chitosan make it easily soluble in acidic solution, but its poor stability limits its application in acidic systems. In order to improve its chemical stability, it is often modified by cross-linking. Commonly used crosslinking agents include formaldehyde, glutaraldehyde, epichlorohydrin, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30
Inventor 肖玲柯蓓蕾云一宁赵业红石金华张昆
Owner WUHAN UNIV
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