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Polyethylene glycol-polyethyleneimine modified ferric oxide nanoparticle preparation method

A nanotechnology of polyethyleneimine and iron oxide, which is applied in the field of materials, can solve the problems of limited application, difficulty in storage, difficulty in water, etc., and achieves the effects of strong operability, uniform particle size distribution, and controllable particle size

Active Publication Date: 2018-07-24
XINYANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is an effective method to modify the surface of iron oxide nanoparticles. For example, polyethyleneimine can be used to modify the surface of iron oxide nanoparticles, but there are still problems of agglomeration, and it is not easy to preserve [Colliods Surf., B ,2014,122,752]
Researchers tried to prepare iron oxide nanoparticles by wet chemical method first, and then modified by polyethyleneimine polymer [J.Magn.Magn.Mater.,2015,375,217], but the obtained polyethyleneimine modified iron oxide nanoparticles Still have disadvantages such as uneven size
Some researchers tried to prepare polyethylene glycol-polyethyleneimine copolymer, and then modified it on the basis of preparing iron oxide nanoparticles by wet chemical method, but the problem of uniform size of nanoparticles has not been effectively improved[Transactions of Nonferrous Metals Society of China, 2008, 18, 393]
Park et al. used high temperature method to prepare iron oxide nanoparticles with uniform size [Nat Mater., 2004,3,891]. However, because the surface of the prepared iron oxide nanoparticles is hydrophobic molecules, it is difficult to easily water, which limits its application in medicine.

Method used

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Effect test

Embodiment 1

[0030] A preparation method of polyethylene glycol-polyethyleneimine modified iron oxide nanoparticles, comprising the following steps:

[0031] 1) 2g polyethylene glycol (M w =1000) was dissolved in 200ml of dichloromethane, 0.2g of maleic anhydride was added, 0.05g of triethylamine and 0.25g of 4-dimethylaminopyridine were added at the same time, reacted at room temperature for 48h, and more than three times the volume of dichloromethane was added The glacial ether precipitation obtains carboxylated polyethylene glycol; Step 1) in, the mol ratio of described polyethylene glycol and maleic anhydride is 1:1; Triethylamine and 4-dimethylaminopyridine mol ratio are 1: 6.28. The total mass of triethylamine and 4-dimethylaminopyridine added is 1.5 times the mass of maleic anhydride.

[0032] 2) 0.4g of the resulting product was dissolved in 40ml of tetrahydrofuran, and 8g of polyethyleneimine (M w =8,000), add 0.05g dicyclohexylcarbodiimide and 0.15g 4-dimethylaminopyridine, rea...

Embodiment 2

[0037] A preparation method of polyethylene glycol-polyethyleneimine modified iron oxide nanoparticles, comprising the following steps:

[0038] 1) 2g polyethylene glycol (M w =1000) was dissolved in 200ml of dichloromethane, 0.25g of maleic anhydride was added, 0.05g of triethylamine and 0.3g of 4-dimethylaminopyridine were added at the same time, reacted at room temperature for 72h, and the carboxyl group was obtained by precipitation with excess glacial ether polyethylene glycol; in step 1), the mol ratio of polyethylene glycol and maleic anhydride is 1:1.28; the mol ratio of triethylamine and 4-dimethylaminopyridine is 1:7.55, triethylamine and The added total mass of 4-dimethylaminopyridine is 1.4 times of the mass of maleic anhydride.

[0039] 2) 0.115g of the resulting product was dissolved in 11.5ml of tetrahydrofuran, and 8g of polyethyleneimine (M w =8,000), add 0.06g dicyclohexylcarbodiimide and 0.17g 4-dimethylaminopyridine, react 72h under room temperature, remo...

Embodiment 3

[0044] A preparation method of polyethylene glycol-polyethyleneimine modified iron oxide nanoparticles, comprising the following steps:

[0045] 1) 2g polyethylene glycol (M w =1000) was dissolved in 200ml of dichloromethane, 0.3g of maleic anhydride was added, 0.1g of triethylamine and 0.4g of 4-dimethylaminopyridine were added at the same time, reacted at room temperature for 60h, and precipitated with excess glacial ether to obtain carboxyl polyethylene glycol; in step 1), the mol ratio of polyethylene glycol and maleic anhydride is 1:1.53; the mol ratio of triethylamine and 4-dimethylaminopyridine is 1:5.03, triethylamine and The total mass added of 4-dimethylaminopyridine is 1.67 times of the mass of maleic anhydride.

[0046] 2) 0.2g of the resulting product was dissolved in 10ml of tetrahydrofuran, and 8g of polyethyleneimine (M w =8,000), add 0.05g dicyclohexylcarbodiimide and 0.15g 4-dimethylaminopyridine, react 96h under room temperature, remove solvent by rotary e...

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Abstract

The invention discloses a polyethylene glycol-polyethyleneimine modified ferric oxide nanoparticle preparation method which comprises the following steps: 1) dissolving polyethylene glycol into dichloromethane, adding maleic anhydride, adding triethylamine and 4-dimethylamino pyridine at the same time, reacting for 48h to 72h under the room temperature condition and adding ice diethyl ether precipitate to obtain a product carboxylated polyethylene glycol; 2) dissolving the product into tetrahydrofuran, adding polyethyleneimine, adding dicyclohexyl carbodiimide and 4-dimehtylamino pyridine, reacting for 72h to 120h under room temperature and performing rotary evaporation to remove a solvent to obtain polyethylene glycol-polyethyleneimine copolymer; 3) obtaining polyethylene glycol-polyethyleneimine modified ferric oxide nanoparticles through a ligand exchange method. The ferric oxide nanoparticles prepared by the preparation method disclosed by the invention has the advantages of even particle size distribution and good water solubility and cytocompatibility.

Description

technical field [0001] The invention belongs to the field of material technology, and in particular relates to a preparation method of polyethylene glycol-polyethyleneimine modified iron oxide nanoparticles. Background technique [0002] Iron oxide nanoparticles (Iron Oxide Nanoparticles) are widely used in magnetic energy storage media, biosensors, drug loading, and medical treatment. In medical treatment applications, the colloidal stability of iron oxide nanoparticles is the main performance index affecting its application [International J.Pharmaceutics.2011,408,130]. It is an effective method to modify the surface of iron oxide nanoparticles. For example, polyethyleneimine can be used to modify the surface of iron oxide nanoparticles, but there are still problems of agglomeration, and it is not easy to preserve [Colliods Surf., B , 2014, 122, 752]. Researchers tried to prepare iron oxide nanoparticles by wet chemical method first, and then modified by polyethyleneimine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06B82Y30/00C08G65/331C08G81/00A61K47/34A61K47/02
CPCA61K47/02A61K47/34B82Y30/00C01G49/06C01P2004/03C08G65/331C08G81/00
Inventor 韩艳婷聂磊谢欣袁红雨孙萌陈世峰董婧李洁郭理想
Owner XINYANG NORMAL UNIVERSITY
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