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Method for preparing narrow-dispersion high-magnetic chitosan sub-micron particles

A chitosan sub- and micro-particle technology is applied in the field of preparation of narrowly dispersed high-magnetic chitosan sub-particles, which can solve the problem that the uniformity of the size and magnetic content of magnetic polymer particles is not easy to control, and it is difficult to meet the requirements of rapid magnetic separation. Surfactant is not easy to remove and other problems, to achieve the effect of narrow dispersion, high magnetic content, and uniform magnetic content

Inactive Publication Date: 2013-04-03
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current problems are: 1) The magnetic content of the obtained magnetic polymer particles is low, mostly less than 25wt%, which is difficult to meet the requirements of fast magnetic separation; 2) The size of each magnetic polymer particle and the uniformity of magnetic content It is not easy to control, which affects the uniformity of the magnetic response; 3) The added surfactant is not easy to remove, and does not take advantage of biomedical applications
However, by these methods, it is difficult to obtain narrowly dispersed magnetic chitosan submicron particles with high magnetic content.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation method of narrowly dispersed highly magnetic chitosan submicron particles, the steps are as follows:

[0018] 1) Add 3.9g FeCl 3 , 7.2g of sodium acetate and 1.2g of sodium citrate were added to 120mL of ethylene glycol, and stirred to dissolve. This solution was transferred to a PTFE-lined reactor with a capacity of 150 mL, sealed and heated to 200 °C for 10 h. The reaction product MCNCs was fully washed with ethanol three times, and dried in vacuum at 60°C for 24 hours to obtain 1.2 g of the product with an average particle size of 250 nm.

[0019] 2) Dissolve 1.0g of chitosan in 320mL of 0.138% acrylic acid aqueous solution, and then disperse 0.8g of MCNCs into this solution to obtain a dispersion.

[0020] 3) Pass N under stirring in the above dispersion 2 After deoxidation, raise the temperature to 70°C, inject 5 mL of an aqueous solution containing 0.22 g of potassium persulfate, and react for 2 h. The reaction temperature was lowered to 40°C, 0....

Embodiment 2

[0023] A preparation method of narrowly dispersed highly magnetic chitosan submicron particles, the steps are as follows:

[0024] 1) Add 3.0g FeCl 3 , 7.2g of sodium acetate and 1.2g of sodium citrate were added to 120mL of ethylene glycol, and stirred to dissolve. This solution was transferred to a PTFE-lined reactor with a capacity of 150 mL, sealed and heated to 200 °C for 10 h. The reaction product MCNCs was fully washed with ethanol three times, and dried under vacuum at 60°C to obtain 0.9 g of the product with an average particle size of 205 nm.

[0025] 2) Dissolve 0.5g of chitosan in 300mL of 0.12% acrylic acid aqueous solution, and then disperse 0.9g of MCNCs into this solution to obtain a dispersion.

[0026] 3) Pass N under stirring in the above dispersion 2 After deoxidation, raise the temperature to 70°C, inject 4 mL of an aqueous solution containing 0.15 g of potassium persulfate, and react for 4 h. The reaction temperature was lowered to 50°C, 0.5 mL of 25%...

Embodiment 3

[0029] A preparation method of narrowly dispersed highly magnetic chitosan submicron particles, the steps are as follows:

[0030] 1) Add 6g FeCl 3 , 10.8g of sodium acetate and 1.8g of sodium citrate were added to 120mL of ethylene glycol, and stirred to dissolve. This solution was transferred to a polytetrafluoroethylene-lined reaction vessel (capacity 150mL), sealed and heated to 200°C for 12h. The reaction product MCNCs was fully washed with ethanol three times, and dried in vacuum at 60°C for 24 hours to obtain 2.0 g of the product with an average particle size of 340 nm.

[0031] 2) Dissolve 1.2g of chitosan in 320mL of 0.2% methacrylic acid aqueous solution, and then disperse 1.2g of MCNCs into this solution to obtain a dispersion.

[0032] 3) Pass N under stirring in the above dispersion 2 After deoxidation, raise the temperature to 70°C, inject 5 mL of an aqueous solution containing 0.15 g of ammonium persulfate, and react for 4 hours. The reaction temperature was...

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Abstract

The invention provides a method for preparing narrow-dispersion high-magnetic chitosan sub-micron particles. The method comprises the following steps: synthesizing sub-micron spherical Fe3O4 colloidal nanocrystal clusters (MCNCs) with carboxylic groups on the surfaces according to a solvothermal method; dispersing the MCNCs in aqueous solution including chitosan and acrylic acid / methacrylic acid; adding initiator, so as to coat chitosan-polyacrylic acid / polymethacrylic acid compound shells on the surfaces of the MCNCs through radical polymerization reaction; adding cross linking agent, so that cross linking reaction is carried out between the MCNCs and part of amino groups in chitosan molecular chains; and finally, washing out polyacrylic acid or polymethacrylic acid with alkali aqueous solution. The method has the advantages that the quantity of organic solvent used during the preparation process is low, so that organic material residue is low; the sizes of magnetic polymer particles depend on those of the pre-prepared MCNCs, so that the regulation and the control are easy, and the particle size distribution is narrow; the magnetic content of the magnetic polymer particles is uniform and high; superparamagnetism is realized; and the method is particularly suitable for being applied to separation, analysis, enzyme immobilization, catalysis and the like.

Description

technical field [0001] The invention relates to the preparation of magnetic materials, in particular to a preparation method of narrowly dispersed highly magnetic chitosan submicron particles. Background technique [0002] Polymer particles containing magnetic materials can use the magnetic properties of their internal cores to achieve rapid magnetic separation or magnetic targeting of particles through an external magnetic field, and can also achieve magnetic heating under an external alternating magnetic field; , on the one hand, it can protect the internal magnetic material from acidic media or oxygen in the air, on the other hand, it can provide functional groups required for specific applications such as coupling ligands, and can also improve its biocompatibility and in Dispersion stability in dispersion media. Magnetic polymer particles have important application prospects in biomedicine and other fields, such as drug controlled release carriers, MRI contrast agents, ...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L51/02C08K3/22C08F251/00C08F220/06
Inventor 傅国旗李义雅柴志华
Owner NANKAI UNIV
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