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Preparation method of water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen

A technology of nano-magnetic particles and iron tetroxide, applied in the field of nano-materials, can solve the problems of limited application, complex synthesis process, hindered application, etc., and achieves the effect of solving monodispersity, simple synthesis method, and easy to expand production.

Inactive Publication Date: 2010-04-21
SHANGHAI NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0002] There are many preparation methods for ferroferric oxide nanoparticles. The traditional method is relatively simple, but the prepared nanomaterial particles are mostly oil-soluble, which needs to be solved by further ligand exchange, polymer coating or silica coating. The functionalization and water solubility of nanoparticles can be used in the biological field, but the complex synthesis process seriously hinders its application in biomedicine
Although silica coating has good dispersibility and water solubility, the process is relatively complicated; organic polymer coating is easy to agglomerate and is not very stable; the method of ligand exchange can solve the problems of the above two methods. defect, the efficiency of ligand exchange has been an intractable problem
At present, the preparation process of biocompatible ferrite magnetic nanoparticles is relatively complicated, and it cannot be prepared in large quantities, which greatly limits the application of such materials in this field.

Method used

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  • Preparation method of water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen
  • Preparation method of water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen
  • Preparation method of water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Weigh FeCl 3 ·6H 2 O (2.720g, 10mmol) and 6-(1,3-dioxoisoindolin-2-yl)hexanoic acid (7.842g, 30mmol) were placed in a 100mL round bottom flask, then 20mL of chloroform and 20ml of water and ethanol, at room temperature, magnetically stirred, 70mmol triethylamine (about 10ml) was added under stirring condition, and stirred for 20-24 hours.

[0028] Wash with water three times, each time with 10ml of water; dry over anhydrous magnesium sulfate for 24 hours, filter with suction, and evaporate the filtrate to dryness to obtain a blood-red oily substance, which is 6-(1,3-dioxoisoindoline-2- base) hexanoic acid iron precursor.

Embodiment 2

[0030]The 6-(1,3-dioxoisoindoline-2-yl) hexanoic acid iron precursor that example 1 obtains is dissolved in 45ml phenyl ether and 15ml oleylamine, pours in the three-necked flask of 250mL, Put the round-bottom flask on the magnetic stirring heater, insert a condenser tube into the middle mouth of the three-necked round-bottom flask, insert a mercury thermometer into one mouth of both sides of the flask to measure the temperature, and connect a nitrogen balloon to the other mouth of the flask. Pour in inert high-purity nitrogen, and at the same time evacuate the flask to form a reflux system.

[0031] After the reaction device is completed, under the condition of magnetic stirring, firstly heat to 120°C-130°C, use nitrogen gas to remove the moisture in the reaction solution, and the heating time is one hour; then raise the temperature to 220°C, under nitrogen protection, and react for half an hour; Then, the temperature was raised to 295°C and refluxed for half an hour to decom...

Embodiment 3

[0034] Take by weighing the oil-soluble Fe of embodiment 2 gained 6-(1,3-dioxoisoindoline-2-yl) hexanoic acid coordination 3 o 4 0.6 g of nanoparticles was dispersed in a mixture of 35 ml of chloroform, 20 ml of absolute ethanol and 15 ml of water, 3 g of hydrazine hydrate was added under stirring conditions, and the mixture was refluxed for 4 hours. After the deamination reaction protected by hydrazine hydrate, the black Fe dispersed in the lower organic phase 3 o 4 The nanoparticles were all transferred to the upper aqueous phase. Centrifuge and wash with ethanol for 3 to 5 times to obtain amino-functionalized water-soluble Fe 3 o 4 Nanoparticles (the organic ligand on the surface is 6-aminocaproic acid) have good monodispersity in water, can be dispersed in water, and are ready for use.

[0035] Its TEM picture is as follows Figure 4 As shown, the average diameter of the obtained iron ferric oxide nanoparticles is 15~25nm; the oil of the 6-(1,3-dioxoisoindoline-2-yl)...

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Abstract

The invention relates to the field of nano materials and discloses a preparation method of a water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen, comprising the following steps of: coordinating carboxyl on n-(1,3-dioxoisoindolin-2-yl) alkyl acid (n is equal to 3-18) with ferrum; pyrolyzing a precursor of n-(1,3-dioxoisoindolin-2-yl) alkyl acid iron at high temperature to obtain an oil-soluble magnetic nanoparticle with lipophilicity and a surface ligand, i.e. the n-(1,3-dioxoisoindolin-2-yl) alkyl acid; then removing phthalic anhydride for protecting amino by a deammoniation protective reagent (hydrazine hydrate) by using a deammoniation protection method, and converting the oil-soluble magnetic nanoparticle into the water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen. The water-soluble ferroferric oxide magnetic nanoparticle with functional amidogen can be excellently dissolved in a water solution and has favorable biocompatibility and paramagnetism.

Description

technical field [0001] The invention relates to the field of nanomaterials, and relates to a synthesis of nano magnetic particles and a preparation method thereof, in particular to the synthesis of an amino-functionalized water-soluble iron ferric oxide nanometer material and its large-scale preparation method and properties. Background technique [0002] There are many preparation methods for ferroferric oxide nanoparticles. The traditional method is relatively simple, but the prepared nanomaterial particles are mostly oil-soluble, which needs to be solved by further ligand exchange, polymer coating or silica coating. The functionalization and water solubility of nanoparticles can be used in the biological field, but the complex synthesis process seriously hinders its application in biomedicine. [0003] Magnetic materials are ancient and widely used functional materials, which are closely related to all aspects of informationization, automation, mechatronics, national defe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/11C01G49/08A61K49/18
Inventor 杨仕平田启威杨红张晶晶
Owner SHANGHAI NORMAL UNIVERSITY
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