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Method for preparing functionalized carbon nanotube based on polyethyleneimine

A polyethyleneimine and carbon nanotube technology is applied in the field of preparation of functionalized carbon nanotubes to achieve the effects of simple preparation process, easy operation and good biocompatibility

Inactive Publication Date: 2009-10-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Retrieval of documents and patents on the surface modification of carbon nanotubes at home and abroad shows that: before the completion of the present invention, carbon nanotubes are further functionalized after surface graft modification and the surface charge of carbon nanotubes after functionalization has a great impact on cells. Toxicity studies have not been systematically reported

Method used

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  • Method for preparing functionalized carbon nanotube based on polyethyleneimine
  • Method for preparing functionalized carbon nanotube based on polyethyleneimine
  • Method for preparing functionalized carbon nanotube based on polyethyleneimine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Configure a mixture of concentrated nitric acid and sulfuric acid with a volume ratio of 3:1 (that is, HNO 3 / H 2 8O 4 is v / v=3:1), carry out acidification treatment to a certain amount of multi-walled carbon nanotubes, after 2 hours, filter, wash with water, and finally place the multi-walled carbon nanotubes after acidification under vacuum condition to dry and store;

[0047] (2) Get 99.8 mg of acidified multi-walled carbon nanotubes in step (1), disperse them in a mixed solution of 20 milliliters of thionyl chloride and 1 milliliter of DMF, and reflux for 24 hours to obtain multi-walled carbon nanotubes containing acid chloride groups on the surface. Reaction product of carbon nanotubes. After the reaction mixture was centrifuged (5000 rpm, 10 minutes) in a high-speed centrifuge, the upper layer solution in the centrifuge tube was poured out. In order to fully remove free thionyl chloride, the centrifuged reaction product should be redispersed in DMF solvent. ...

Embodiment 2

[0051] Take 30 mg of the CNT / PEI carbon nanotubes in Example 1 in a 20 ml vial, add 5 ml of DMSO solvent, and stir magnetically to make it evenly dispersed. Subsequently, 5 ml of DMSO solution containing 410 mg of succinic anhydride was added, and the carboxylation reaction was carried out for 24 hours under strong magnetic stirring. In order to ensure that succinic anhydride and the PEI polymer on the CNT / PEI complex are covalently bonded, we dialyzed the reacted mixture with pure water (3 times, 4 liters) for 3 days with a dialysis membrane of MWCO=50000. Remove the DMF solvent, excess reagents and small molecule by-products produced during the reaction in the reaction mixture. Finally, the purified product CNT / PEI.SAH is freeze-dried to obtain functionalized multi-walled carbon nanotubes with negative surface charges. NMR test shows that the amino group of PEI polymer modified on the surface of multi-walled carbon nanotubes has been successfully converted into the end grou...

Embodiment 3

[0053] (1) Take concentrated nitric acid, acidify a certain amount of single-walled carbon nanotubes, after 3 hours, filter, wash with water, and finally place the acidified single-walled carbon nanotubes under vacuum conditions for drying and then preserve;

[0054](2) Get 105 mg of acidified single-walled carbon nanotubes in step (1), disperse them in a mixed solution of 25 milliliters of thionyl chloride and 1 milliliter of DMF, and reflux for 30 hours to obtain single-walled carbon nanotubes containing acid chloride groups on the surface. Reaction product of carbon nanotubes. After the reaction mixture was centrifuged (5000 rpm, 10 minutes) in a high-speed centrifuge, the upper layer solution in the centrifuge tube was poured out. In order to fully remove free thionyl chloride, the centrifuged reaction product should be redispersed in DMF solvent. And centrifuged again, repeating this 5 times, the last purified single-walled carbon nanotubes containing acid chloride groups...

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Abstract

The invention relates to a method for preparing a functionalized carbon nanotube based on a polyethyleneimine, comprising the following steps of: (1) dipping the carbon nanotube in a strong acid for 2-4 hours, subsequently filtering, drying and storing the carbon nanotube; (2) conducting the circumfluence operation in the DMF of SOCl2 and introducing acyl chloride on the surface of the carbon nanotube and subsequently centrifuging and washing the carbon nanotube by the DMF; (3) dispersing the carbon nanotube in the DMF solvent and adding the DMF solution with PEI dissolved wherein; mixing the mixed solution by strong magnetic force; subsequently adding tri-ethylamine in the solution; repeatedly conducting a plurality of pure water dialysis after reaction; subsequently obtaining the CNT / PEI by freezing and drying; and (4) conducting acetylation reaction on the amino functional group on the surface of the CNI / PEI; or conducting carboxyl reaction on the amido on the surface of the CNT / PEI. The method has simple preparation process, moderate reaction condition, easy operation and industrial executive prospect; and the carbon nanotube prepared by the method can be dispersed in the solution for long, the agglomeration phenomenon does not occur and the carbon nanotube has excellent biocompatibility and safety in bio-medicals.

Description

technical field [0001] The invention belongs to the field of preparation of functionalized carbon nanotubes, in particular to a method for preparing functionalized carbon nanotubes mediated by polyethyleneimine. Background technique [0002] As one of the most representative nanomaterials, carbon nanotubes have demonstrated their unique properties in composite reinforced nanomaterials, The huge application potential in the fields of semiconductor materials, catalyst carriers, and biomedical materials has also been favored by researchers from all walks of life. With the expansion of research on the application of carbon nanotubes, it is found that due to the small size effect, surface effect and high surface free energy of nanoparticles, carbon nanotubes are very easy to form large aggregates, and the dispersion performance in solution is poor. , greatly restricting its further development and application in many fields. [0003] For this reason, improving the ease of agglo...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 史向阳沈明武肖仕丽
Owner DONGHUA UNIV
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