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Magnetic polymer based on polyethyleneimine and its preparation method

A polyethyleneimine and polymer technology, which is applied in the field of polyethyleneimine-based magnetic polymers and their preparation, can solve the problems of complex process, high cost, poor compatibility and the like, and achieves simple process, low cost and stable performance. strong effect

Inactive Publication Date: 2016-05-11
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former has the problem of poor compatibility, while the latter is often complicated in process and high in cost
The synthesis method of magnetic polymer with simple preparation process, relatively low cost and controllable magnetic properties is still blank

Method used

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  • Magnetic polymer based on polyethyleneimine and its preparation method
  • Magnetic polymer based on polyethyleneimine and its preparation method
  • Magnetic polymer based on polyethyleneimine and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] magnetic polymer A 1 Synthesis:

[0026]

[0027] (1) Dissolve linear PEI (270.8 mg, 6.3 mmol) with a molecular weight of 600 Da in 5 ml of absolute ethanol, and add dropwise into iodomethane (4 ml, 64.2 mmol). Stir at 42° C. for 60 h, centrifuge after the reaction to obtain a yellow solid which is dissolved in water, precipitate in ethanol, centrifuge, and vacuum-dry to obtain the intermediate product 1a.

[0028] (2) Dissolve 1a (146.0 mg, 1.0 mmol) in water, add 4 g of chloride ion exchange resin to the system and stir for 8 h. After filtration, the filtrate was rotary evaporated and dried in vacuo to obtain light yellow solid 1b. According to the elemental analysis in Table 1, the quaternization conversion rate was 66%. Such as figure 1 Shown is the H NMR spectrum of 1b, 1 HNMR (500Hz,D 2 O) Chemical shift δ: 3.2-3.6 (multiple peaks, -CH connected to the quaternization unit 2 -, -CH 3 ), 2.7-3.2 (multiplet, -CH connected to PEI unit 2 -).

[0029] (3) 1b...

Embodiment 2

[0031] magnetic polymer A 2 Synthesis:

[0032]

[0033] (1) Dissolve linear PEI (268.7 mg, 6.2 mmol) with a molecular weight of 1000 kDa in 5 ml of absolute ethanol, and add dropwise into iodomethane (3.9 ml, 62.6 mmol). Stir at 50° C. for 100 h, centrifuge after the reaction to obtain a yellow solid which is dissolved in water, precipitate in ethanol, centrifuge, and vacuum-dry to obtain the intermediate product 2a.

[0034] (2) Dissolve 2a (175.6mg, 1.0mmol) in water, add 4g of chloride ion exchange resin to the system and stir for 12h. After filtration, the filtrate was rotary evaporated and dried in vacuo to obtain light yellow solid 2b. According to the elemental analysis in Table 1, the quaternization conversion rate was 85%.

[0035] (3) 2b (83.2mg, 1.0mmol) and FeCl equivalent to the quaternization unit 3 ·6H 2O (170.4mg, 0.633mmol) was dissolved in 5ml of methanol, stirred for 24h, suspended and evaporated, the product was washed with anhydrous ether, centrifu...

Embodiment 3

[0037] magnetic polymer A 3 Synthesis:

[0038]

[0039] (1) Linear PEI (268.7mg, 6.2mmol) with a molecular weight of 10kDa was dissolved in 5ml of absolute ethanol, and added dropwise to iodomethane (0.23ml, 0.37mmol). Stirring at 20° C. for 1 h, after the reaction was completed, centrifuged to obtain a yellow solid which was dissolved in water, precipitated in ethanol, centrifuged, and dried in vacuo to obtain the intermediate product 3a.

[0040] (2) Dissolve 3a (82.1mg, 1.0mmol) in water, add 4g of chloride ion exchange resin to the system and stir for 12h. After filtration, the filtrate was rotary evaporated and dried in vacuo to obtain light yellow solid 3b. According to the elemental analysis in Table 1, the quaternization conversion rate was 25%.

[0041] (3) 3b (59.1mg, 1.0mmol) and FeCl equivalent to the quaternization unit 3 ·6H 2 O (170.4mg, 0.633mmol) was dissolved in 5ml of methanol, stirred for 24h, suspended and evaporated, the product was washed with an...

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Abstract

The invention relates to magnetic polymer based on polyethyleneimine and a preparation method of the magnetic polymer. According to the preparation method, linear and branched polyethyleneimines are utilized as macromolecular reactants, and modification is carried out to synthesize the magnetic polymer. The preparation method concretely comprises the following steps: carrying out quaterisation on polyethyleneimine, carrying out ion exchang, replacing original anions by using four ferrous halogen anions to synthesize a main chain type magnetic polymer with a magnetic primitive element. According to the magnetic polymer disclosed by the invention, the molecular weight of PEI used by the polymer is 600Da-1000kDa, and Fe / N is 0.25-0.85. According to the preparation method disclosed by the invention, polyethyleneimines with different chain structures and molecular weights react with and methyl iodide to generate quaternary ammonium salts, and the quaternary ammonium salts are subjected to ion exchange and then react with metal halide to synthesize the polymer with the magnetic primitive element. The preparation method has the advantages of low cost, simple and convenient process, mild reaction conditions, simple operation steps and the like. The magnetic polymer has potential applications in the aspects of magnetic film materials, electromagnetic devices, wave absorbing materials, CO2 separation and adsorption and the like.

Description

technical field [0001] The present invention relates to a class of magnetic polymers and their synthesis methods, in particular to polyethyleneimine-based magnetic polymers and their preparation methods; linear and branched polyethyleneimines (PEI) are used as macromolecular reactants for post-modification synthesis Magnetic polymer approach. Background technique [0002] As the macromolecule with the highest density of amino groups, polyethyleneimine (PEI) has unique physical and chemical properties, so it has attracted a lot of researchers' interest in it. Boussif et al. (Boussif et al., Proceeding of the National Academy of Sciences, 92 (16), 7297-7301.) found that PEI can be used as a gene transfection reagent. Beyth et al. (Beythetal. Biomaterials 27 (2006) 3995-4002.) mixed cross-linked quaternized PEI into medical resin to study its antibacterial effect. Hu (Huetal., The Journal of Physical Chemistry B, 2005, 109(10): 4285-4289.) et al. used PEI to modify carbon nan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/04
Inventor 任丽霞于小龙袁晓燕
Owner TIANJIN UNIV
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