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Temperature-controlled pressure-controlled microwave synthesis method for water-soluble ferroferric oxide nano crystal

A technology of ferroferric oxide and nanocrystals, applied in chemical instruments and methods, iron oxide/iron hydroxide, crystal growth, etc., can solve problems such as good monodispersity, achieve good water solubility and stability, and can be sized Tuning and operation are simple

Inactive Publication Date: 2008-04-16
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to aim at the defects of the current aqueous phase and organic phase synthesis methods, to provide a temperature-controlled and pressure-controlled microwave synthesis method of water-soluble ferric oxide nanocrystals, which has the advantages of fast synthesis speed, good water solubility and monodispersity good advantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1. Preparation of reaction precursor solution:

[0016] Dissolve ferrous chloride and ferric chloride with a molar ratio of 1:2 in water, the total iron concentration is 0.01 mol / liter, add glycerol as a stabilizer, and control the volume ratio of glycerol to water at 1:1 . Adjust the pH of the solution to 12 to obtain a precursor solution.

[0017] 2. Microwave synthesis of ferric oxide nanocrystals:

[0018] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate ferric oxide nanocrystals.

[0019] The microwave heating conditions are:

[0020] Microwave oscillation frequency: 2450MHZ,

[0021] Microwave power: 400W,

[0022] Heating time: 4 hours,

[0023] Heating temperature: 140 degrees Celsius.

Embodiment 2

[0025] 1. Preparation of reaction precursor solution:

[0026] Dissolve ferrous sulfate and ferric sulfate with a molar ratio of 1:2 in water, the total iron concentration is 0.04 mol / liter, add 1,2-propanediol as a stabilizer, and control the volume ratio of 1,2-propanediol to water at 1 : 2. Adjust the pH of the solution to 8 to obtain a precursor solution.

[0027] 2. Microwave synthesis of ferric oxide nanocrystals:

[0028] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate ferric oxide nanocrystals.

[0029] The microwave heating conditions are:

[0030] Microwave oscillation frequency: 2450MHZ,

[0031] Microwave power: 600W,

[0032] Heating time: 30 minutes,

[0033] Heating temperature: 160 degrees Celsius.

Embodiment 3

[0035] 1. Preparation of reaction precursor solution:

[0036] Dissolve ferrous nitrate and ferric nitrate with a molar ratio of 1:2 in water, the total iron concentration is 0.1 mol / liter, add ethylene glycol as a stabilizer, and control the volume ratio of ethylene glycol to water at 1:4. Adjust the pH of the solution to 10 to obtain a precursor solution.

[0037] 2. Microwave synthesis of ferric oxide nanocrystals:

[0038] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate ferric oxide nanocrystals.

[0039] The microwave heating conditions are:

[0040] Microwave oscillation frequency: 2450MHZ,

[0041] Microwave power: 100W,

[0042] Heating time: 2 hours,

[0043] Heating temperature: 200 degrees Celsius.

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Abstract

This invention relates to a method for synthesizing water-soluble ferroferric oxide nanocrystal by temperature and pressure controlled microwave. Wherein: use water as solvent, ferrous and ferric salt as raw material, water-soluble polyatomic alcohol as stabilizer, adjust the solution pH to produce the basic precursor reaction solution, and then put this precursor solution in closed polytetrafluoroethylene tank,the reaction is conducted in temperature and pressure controlled microwave reactor to quickly synthesize the ferroferric oxide nanocrystal. This invented method is characterized of simple operation, mild conditions, and low cost. Besides, the synthesized product ferroferric oxide nanocrystal is characterized of good water-solubility and stability, strong magnetic property, homogeneous dimension distribution, adjustable size and easy conjunction with biological macromolecules.

Description

technical field [0001] The invention relates to a temperature-controlled and pressure-controlled microwave synthesis method for water-soluble iron ferric oxide nanocrystals. Ferric iron tetroxide magnetic nanocrystals are prepared using temperature-controlled and pressure-controlled microwave synthesis techniques using trivalent and divalent iron salts as raw materials. , belongs to the technical field of nanomaterial preparation. Background technique [0002] Fe 3 o 4 The bulk material is a ferromagnetic compound. When nano-Fe 3 o 4 When the particle size is about 3-10 nanometers, due to the scale quantum effect and the dielectric confinement effect, they exhibit superparamagnetic properties (that is, they are magnetic in the presence of a magnetic field and non-magnetic when the magnetic field disappears). This material with special properties has a wide range of applications in nuclear magnetic resonance imaging, targeted drug therapy, separation of biomolecules and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08C30B7/00
CPCC30B7/00
Inventor 任吉存李良
Owner SHANGHAI JIAOTONG UNIV