Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles

A magnetic nanoparticle, nanoparticle technology, applied in ferrous oxide, iron oxide/iron hydroxide, nanotechnology, etc.

Inactive Publication Date: 2011-10-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Retrieve Fe related to APTS protection at home and abroad 3 o 4 Literature and patent results on nanoparticle synthesis show that APTS-protected Fe 3 o 4 Nanoparticle research has not yet been reported

Method used

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  • Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles
  • Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles
  • Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) 1.25g FeCl 2 4H 2 O was sonicated with 7.5 mL of ultrapure water, and then 6.5 mL of NH 3 ·H 2 O was stirred in air for 10 min, then 2.5 mL of 3-aminopropyltriethoxysilane (APTS) was added, and reacted in an autoclave at 134 ° C for 3 hours;

[0048] (2) After the reaction finishes, cool down to room temperature naturally, and the obtained black precipitate Fe 3 o 4 / APTS is dispersed in ethanol or ultrapure water, magnetically separated, redispersed, and magnetically separated, and washed twice with ethanol and five times with pure water to remove excess reagents and redispersed in the water phase.

[0049] TEM test results showed that Fe 3 o 4 The morphology, size and size distribution of / APTS nanoparticles were calculated by Fe 3 o 4 / APTS has a particle size of 6.5nm and no Fe was found3 o 4 / APTS nanoparticles aggregation, indicating that APTS is uniformly modified on the Fe 3 o 4 on the surface of nanoparticles.

Embodiment 2

[0051] (1) 2g FeCl 2 4H 2 O was sonicated with 12 mL of ultrapure water, and then 10 mL of NH 3 ·H 2 O was stirred in air for 10 min, then added 4 mL of 3-aminopropyltriethoxysilane (APTS), and reacted in an autoclave at 140° C. for 5 hours;

[0052] (2) After the reaction finishes, cool down to room temperature naturally, and the obtained black precipitate Fe 3 o 4 / APTS is dispersed in ethanol or ultra-pure water, magnetically separated, re-dispersed, and magnetically separated, and washed twice with ethanol and five times with pure water to remove excess reagents and re-dispersed in the water phase.

[0053] TEM test results showed that Fe 3 o 4 The morphology, size and size distribution of / APTS nanoparticles were calculated by Fe 3 o 4 The particle size of / APTS is 6.7nm, and Fe is not found 3 o 4 / APTS nanoparticles aggregation, indicating that APTS is uniformly modified on the Fe 3 o 4 on the surface of nanoparticles.

Embodiment 3

[0055] (1) The Fe prepared by one-step method 3 o 4 / APTS nanoparticles were dispersed in 10mL of ultrapure water, mixed well with 9.8μL of triethylamine solution, then added dropwise to 1mL of methanol solution containing 7.2mg of acetic anhydride, reacted for 24 hours under strong magnetic stirring, and the surface charge was obtained. Sexual Fe 3 o 4 / APTS.Ac nanoparticles;

[0056] (4) Fe prepared in step (2) 3 o 4 / APTS nanoparticles were dispersed in 5 mL DMSO, and 5 mL of DMSO solution containing 10 mg succinic anhydride (-SAH / -NH 2 molar ratio=5:1), reacted for 24 hours under strong magnetic stirring, centrifuged and washed four times, and the surface was negatively charged Fe 3 o 4 / APTS.SAH nanoparticles;

[0057] Zeta surface potential measurements showed that after acetylation and carboxylation reactions, Fe 3 o 4 / APTS.Ac and Fe 3 o 4 / APTS.SAH surface potential from the initial Fe 3 o 4 The +26.7mV of / APTS dropped to -3.2mV and -25.6mV, respectivel...

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Abstract

The invention relates to a preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles. The preparation method comprises the following steps of: (1) mixing an Fe source with ultrapure water, then adding NH3.H2O, stirring in air, then adding 3-aminopropyltriethoxysilane, reacting at the temperature of 134-140 DEG C for 3-5 hours, wherein the volume ratio of 3-aminopropyltriethoxysilane to ultrapure water is 1:3; naturally cooling to room temperature after reaction, and washing and separating precipitate to obtain Fe3O4 / APTS; and (2) carrying out acetylation and carboxylation on Fe3O4 / APTS. The preparation method has the characteristics of simple process, mild reaction conditions and easiness in operation and separation; and the prepared iron oxide magnetic nanoparticles can be dispersed in a water-based solution for a long time without agglomeration phenomenon and can be potentially applied to MRI (magnetic resonance imaging) diagnosis.

Description

technical field [0001] The invention belongs to the field of preparation of iron oxide magnetic nanoparticles, in particular to a preparation method of APTS-modified iron oxide magnetic nanoparticles. Background technique [0002] In recent years, because of their strong magnetic anisotropy, Fe3O4 magnetic nanoparticles (MNPs) have been widely used in various biomedical fields, such as magnetically controlled anticancer drug delivery, hyperthermia magnetic resonance imaging (MRI) . It is well known that the particle size and surface chemical structure of MNPs are critical to their properties and functions in vivo, such as half-life in blood circulation, pharmacokinetics, and biological distribution. Typically, the size of the nanoparticles is controlled by taking appropriate synthetic methods or / and adding surfactants during the reaction to control the crystal growth process. At present, the commonly used synthesis methods for the synthesis of several to tens of nanometer-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82Y40/00
Inventor 沈明武蔡红东史向阳
Owner DONGHUA UNIV
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