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A kind of preparation method of adipate dihydrazide cross-linked carboxymethyl chitosan microspheres

A technology of carboxymethyl chitosan microspheres and adipic acid dihydrazide is applied in the fields of biological materials and environmental protection, and can solve the problems of reduced adsorption performance, difficult recovery, easy loss, etc., and achieves improved adsorption capacity and a simple method. , the effect of uniform particle size

Active Publication Date: 2018-03-16
OCEAN UNIV OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, carboxymethyl chitosan, like chitosan, has the disadvantages of easy loss and difficult recovery during application.
In this regard, the traditional solution is to prepare microspheres by cross-linking carboxymethyl chitosan with glutaraldehyde, formaldehyde, epichlorohydrin, etc. to reduce loss and facilitate recovery, but these cross-linking agents will occupy carboxymethyl chitosan. Adsorption sites of base chitosan, reducing its adsorption performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1g carboxymethyl chitosan (80% carboxylation degree) was dissolved in 20mL distilled water, adjusted to pH=4 with 0.1mol / L HCl, as the water phase; 1.8mL Span-80 was added to 90mL liquid paraffin, as the oil phase; 0.2 g of adipic dihydrazide and 0.25 g of EDC·HCl were dissolved in 9 mL of distilled water to prepare a mixed solution. Keeping the temperature at 20°C, add the prepared water phase drop by drop into the continuously stirring oil phase at a stirring speed of 700 r / min, and continue stirring for 30 min after the dropping is completed. Add the prepared mixed solution of adipic acid dihydrazide and EDC·HCl, continue to stir for 5 hours, separate, wash and dry the obtained product, and prepare adipic acid dihydrazide cross-linked carboxymethyl chitosan microspheres.

Embodiment 2

[0025] 3g carboxymethyl chitosan (carboxylation degree 75%) was dissolved in 75mL distilled water, adjusted pH=4.5 with 0.1mol / L HCl, as the water phase; 9mL Span-80 was added to 300mL liquid paraffin, as the oil phase; 0.35 1 g of adipic acid dihydrazide and 0.38 g of EDC·HCl were dissolved in 13 mL of distilled water to prepare a mixed solution. Keeping the temperature at 25°C, add the prepared water phase drop by drop into the continuously stirring oil phase at a stirring speed of 600r / min, and continue stirring for 50 min after the dropping is completed. Add the prepared mixed solution of adipic acid dihydrazide and EDC·HCl, continue to stir for 4 hours, separate, wash and dry the obtained product, and prepare adipic acid dihydrazide cross-linked carboxymethyl chitosan microspheres.

Embodiment 3

[0027] Dissolve 0.5g carboxymethyl chitosan (carboxylation degree 75%) in 11mL distilled water, adjust pH=4 with 0.1mol / L HCl, as the water phase; add 1.1mL Tween-80 to 55mL liquid paraffin, as the oil phase ; 0.14g of adipic acid dihydrazide and 0.14g of EDC·HCl were dissolved in 4mL of distilled water to prepare a mixed solution. Keeping the temperature at 25°C, add the prepared water phase dropwise to the continuously stirring oil phase at a stirring speed of 900 r / min, and continue stirring for 60 min after the dropping is completed. Add the prepared mixed solution of adipic acid dihydrazide and EDC·HCl, continue to stir for 6 hours, separate, wash and dry the obtained product, and prepare adipic acid dihydrazide cross-linked carboxymethyl chitosan microspheres.

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PUM

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Abstract

The invention relates to a preparation method of adipic acid dihydrazide cross-linked carboxymethyl chitosan microspheres, which belongs to the field of biological materials and environmental protection. Acid dihydrazide is used as a cross-linking agent, and the microspheres are prepared by emulsification cross-linking method, and multiple imino groups are introduced at the same time, which can chelate heavy metal ions, overcome the defect that traditional cross-linking agents will occupy the adsorption sites, and effectively improve the The adsorption capacity of the microspheres; the method is simple, the preparation process is stable, and the prepared microspheres are spherical and uniform in particle size. The microspheres prepared by the invention are stable in acidic, neutral and alkaline water environments, have good mechanical properties, and have good application prospects in the field of heavy metal ion adsorption. Therefore, the technology of the present invention has strong economic development potential.

Description

technical field [0001] The invention belongs to the field of biological materials and environmental protection, and relates to a preparation method of adipic acid dihydrazide cross-linked carboxymethyl chitosan microspheres. Background technique [0002] Because carboxymethyl chitosan contains a large number of active groups such as amino, hydroxyl and carboxyl groups, it can bind heavy metal ions through chelation and charge attraction, so it can be used as an adsorbent for heavy metal ions. Biocompatibility and biodegradability, will not cause secondary pollution to the environment. However, carboxymethyl chitosan is easily soluble in water, so it will be lost in a neutral water environment. Therefore, carboxymethyl chitosan, like chitosan, has the disadvantages of easy loss and difficult recovery during application. In this regard, the traditional solution is to prepare microspheres by cross-linking carboxymethyl chitosan with glutaraldehyde, formaldehyde, epichlorohydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/22C08L5/08
Inventor 刘成圣党奇峰郑恩东高辉范冰
Owner OCEAN UNIV OF CHINA
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