Water-soluble monodisperse iron-nickel magnetic nanoparticles and application thereof
A magnetic nanoparticle, monodisperse technology, applied in the direction of nuclear magnetic resonance / magnetic resonance imaging contrast agent, emulsion delivery, drug delivery, etc., to achieve the effect of good water solubility, low price and strong relaxation ability
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Embodiment 1
[0035] Weigh NiCl 2 .6H 2 O (2.377g, 10mmol) was dissolved in 10ml of water, then acetylacetone (4.1ml, 40mmol) was added to the reaction solution, under room temperature, magnetically stirred, after 15min, the stirring was stopped, and 3ml of triethylamine was added to the reaction solution. A large green precipitate will appear, filter.
[0036] Then prepare a mixed solution of ethanol and water (the volume ratio of ethanol and water is 8: 2), add the obtained green solid to the solution, stir at a temperature of 90°C until it is completely dissolved, then cool at room temperature, and find that Green flaky crystals, filtered, the green flaky crystals obtained are the desired product Ni(acac) 2 .
Embodiment 2
[0038] Weigh FeCl 3 (1.62g, 10mmol) was dissolved in 10ml of water, then added acetylacetone (6.15ml, 60mmol) in the reaction solution, under the condition of room temperature, magnetic stirring, stop stirring after 15min, add 3ml triethylamine, the reaction solution will A large amount of red precipitate appeared and was filtered.
[0039] Then prepare a mixed solution of ethanol and water (the volume ratio of ethanol to water is 7:3), add the obtained red solid to this solution, stir at a temperature of 80°C until it is completely dissolved, then cool at room temperature, and filter to obtain The red granular crystal is the desired product Fe(acac) 3 .
Embodiment 3
[0041] Take the prepared Fe(acac) of embodiment 1 and 2 3 (0.75mmol, 0.2647g) and Ni(acac) 2 (2.25mmol, 0.5775g), was added to a 100ml three-necked flask, and oil amine (20mL, 75.5%) was added to a 100ml three-necked flask.
[0042] Under the condition of magnetic stirring, first heated to 130°C with N 2 Drain the water and air in the reaction solution, maintain the nitrogen protection state, heat for 0.5h; then raise the temperature to 300°C and reflux for 1h; stop stirring, cool to room temperature, centrifuge, and use absolute ethanol and cyclohexane with a volume ratio of 1: The mixed solution of 1 (can be mixed in any volume ratio) was washed 3 to 5 times to obtain a black substance, which was dried in vacuum. This black substance is oil-soluble FeNi whose surface is oleylamine 3 magnetic nanoparticles.
[0043] Tested by JEOL JEM-2100 High Resolution Transmission Electron Microscope (HR-TEM), the obtained Transmission Electron Microscope (TEM) photos and High Resolut...
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