CN103274475B - Preparation method of castor oil coated magnetic iron oxide nanoparticles - Google Patents
Preparation method of castor oil coated magnetic iron oxide nanoparticles Download PDFInfo
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- CN103274475B CN103274475B CN201310218720.0A CN201310218720A CN103274475B CN 103274475 B CN103274475 B CN 103274475B CN 201310218720 A CN201310218720 A CN 201310218720A CN 103274475 B CN103274475 B CN 103274475B
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Abstract
The invention discloses a preparation method of castor oil coated magnetic iron oxide nanoparticles, which comprises the following steps: adding 1 part by weight of iron salt mixture into 10-50 parts by weight of alcohol, stirring for 5-120 minutes, and sufficiently dissolving to obtain an iron salt-containing alcohol solution; adding 80-200 parts by weight of castor oil, stirring for 30-120 minutes, heating to 75-95 DEG C, and refluxing for 30-120 minutes to obtain an iron salt-containing castor oil solution; and adding 5-10 parts by weight of alkaline solution, further stirring at 75-180 DEG C for 0.1-5 hours, cooling to room temperature, performing centrifugal separation, washing with ethanol, and drying at 60 DEG C for 12 hours to obtain magnetic iron oxide nanoparticles. According to the invention, the method has the advantages of accessible raw materials, mild reaction, simple operation, convenient separation, excellent superparamagnetism, high synthesis safety, low environmental pollution and the like; and the prepared nanoparticles has wide application prospects in the aspects of adsorption, biological separation, magnetic catalysis and the like.
Description
Technical field
The invention belongs to magnetic Nano material technical field, particularly the preparation method of the coated superparamag-netic iron oxide of a kind of castor oil.
Background technology
Magnetic ferric oxide nano material is a kind of application functional material very widely; The magnetic ferric oxide nano particles that is less than 20 nm at room temperature has superparamagnetism, under the effect of outside magnetic field, produces magnetic response; According to these characteristics, magnetic ferric oxide nano particles has demonstrated tempting application prospect at aspects such as Magnetic Isolation, magnetic monitoring, magnetic resonance imaging, medicine releases; At present, report prepared by existing more relevant magnetic ferric oxide nano particles, but utilize this crude vegetal of castor oil to prepare the also rarely seen report of superparamag-netic iron oxide; Due to castor oil, have the features such as wide material sources, low price, good biocompatibility, with it, for stabilizer is prepared superparamag-netic iron oxide, can to realize the low cost of ferric oxide nano particles synthetic; Meanwhile, owing to there being castor oil to be coated on the surface of ferric oxide nanometer particle, give ferric oxide nanometer particle continue functionization required reactive group, greatly improved the biocompatibility of superparamag-netic iron oxide.
Summary of the invention
The preparation method who the object of this invention is to provide the coated superparamag-netic iron oxide of a kind of castor oil, this preparation method utilizes castor oil to make stabilizer, has made distribution of sizes little, the superparamag-netic iron oxide of magnetic property excellence.
Concrete steps are:
(1) the molysite mixture of 1 weight portion is joined in the alcohol of 10 ~ 50 weight portions, stir and it was fully dissolved in 5 ~ 120 minutes, make the alcoholic solution that contains molysite.
(2) castor oil that adds 80 ~ 200 weight portions in the alcoholic solution that contains molysite making to step (1), stirs 30 ~ 120 minutes, then is heated to 75 ~ 95 ℃ of backflows 30 ~ 120 minutes, makes the castor oil solution that contains molysite.
(3) alkaline solution that adds 5 ~ 10 weight portions in the castor oil solution that contains molysite making to step (2), at 75 ~ 180 ℃, continue to stir 0.1 ~ 5 hour, then cool to room temperature, after centrifugation ethanol washs 3 ~ 4 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described molysite mixture is the mixture of trivalent iron salt and divalent iron salt, and wherein the mol ratio of trivalent iron salt and divalent iron salt is 2:1, and trivalent iron salt is a kind of in iron chloride, ferric nitrate and ferric sulfate, and divalent iron salt is frerrous chloride.
Described alcohol is a kind of in ethanol, methyl alcohol, ethylene glycol, diethylene glycol (DEG) and glycerol.
Described alkaline solution be amount of substance concentration be 4 mol/L ammoniacal liquor, NaOH ethanolic solution and potassium hydroxide-ethanol solution in a kind of.
Described chemical reagent is chemical pure and above purity.
The prepared superparamag-netic iron oxide of the inventive method has been tested its magnetic property with vibrating specimen magnetometer, and result shows that it has good superparamagnetic performance; With transmission electron microscope and X-ray diffraction, tested its size and structure, found that it is that size is at the ferric oxide nanometer particle of 4 ~ 8 nanometers; With thermogravimetic analysis (TGA) and examination of infrared spectrum its surface composition, confirmed that its surface contains castor oil molecule.
In addition, preparation method of the present invention has that raw material is easy to get, reaction temperature with, simple to operate, be convenient to the advantages such as separated, synthetic safe and environmental pollution is little, prepared superparamag-netic iron oxide has good application prospect at aspects such as absorption, bio-separation and magnetic catalysis.
Accompanying drawing explanation
Fig. 1 is that the coated superparamag-netic iron oxide of castor oil of the embodiment of the present invention 1 preparation shows the photo of magnetic property under magnetic field condition.
Fig. 2 is the coated superparamag-netic iron oxide of the castor oil of the embodiment of the present invention 1 preparation magnetic hysteresis loop at room temperature.
Fig. 3 is the transmission electron microscope figure of the coated superparamag-netic iron oxide of the castor oil of the embodiment of the present invention 1 preparation.
Fig. 4 is the x-ray diffraction pattern of the coated superparamag-netic iron oxide of the castor oil of the embodiment of the present invention 1 preparation.
Fig. 5 is the infrared spectrogram of the coated superparamag-netic iron oxide of the castor oil of the embodiment of the present invention 1 preparation.
Fig. 6 is the thermogravimetric curve figure of the coated superparamag-netic iron oxide of the castor oil of the embodiment of the present invention 1 preparation.
Embodiment
embodiment 1:
(1) 0.37 gram of molysite mixture (mixture of 1 mM of iron chloride and 0.5 mM of frerrous chloride) is joined in 6.32 grams of ethanol, stir and it was fully dissolved in 30 minutes, make the ethanolic solution that contains molysite.
(2) in the ethanolic solution that contains molysite making to step (1), add the castor oil of 38.76 grams, stir 30 minutes, then be heated to 90 ℃ of backflows 30 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, adding 1.85 grams of concentration is the ammonia spirit of 4 mol/L, at 90 ℃, continue to stir 2 hours, then cool to room temperature, after centrifugation ethanol washs 3 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
embodiment 2:
(1) 0.25 gram of molysite mixture (mixture of 0.5 mM of ferric nitrate and 0.25 mM of frerrous chloride) is joined in 6.25 grams of methyl alcohol, stir and it was fully dissolved in 5 minutes, make the methanol solution that contains molysite.
(2) in the methanol solution that contains molysite making to step (1), add 28.25 grams of castor oil, stir 60 minutes, then be heated to 75 ℃ of backflows 120 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, add the NaOH ethanolic solution that 1.75 grams of concentration are 4 mol/L, at 75 ℃, continue to stir 5 hours, then cool to room temperature, after centrifugation ethanol washs 4 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
embodiment 3:
(1) 0.18 gram of molysite mixture (mixture of 0.5 mM of iron chloride and 0.25 mM of frerrous chloride) is joined in 6.3 grams of ethylene glycol, stir and it was fully dissolved in 60 minutes, make the ethylene glycol solution that contains molysite.
(2) in the ethylene glycol solution that contains molysite making to step (1), add 31.14 grams of castor oil, stir 120 minutes, then be heated to 95 ℃ of backflows 120 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, adding 1.35 grams of concentration is the potassium hydroxide-ethanol solution of 4 mol/L, at 180 ℃, continue to stir 0.1 hour, then cool to room temperature, after centrifugation ethanol washs 4 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
embodiment 4:
(1) 0.10 gram of molysite mixture (mixture of 0.2 mM of ferric sulfate and 0.1 mM of frerrous chloride) is joined in 4.5 grams of diethylene glycol (DEG)s, stir and it was fully dissolved in 120 minutes, make the diethylene glycol solution that contains molysite.
(2) in the diethylene glycol solution that contains molysite making to step (1), add 15.5 grams of castor oil, stir 120 minutes, then be heated to 90 ℃ of backflows 120 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, adding 0.85 gram of concentration is the ammonia spirit of 4 mol/L, at 150 ℃, continue to stir 0.5 hour, then cool to room temperature, after centrifugation ethanol washs 3 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
embodiment 5:
(1) 0.37 gram of molysite mixture (mixture of 1 mM of iron chloride and 0.5 mM of frerrous chloride) is joined in 18.5 grams of glycerol, stir and it was fully dissolved in 45 minutes, make the glycerol solution that contains molysite.
(2) in the glycerol solution that contains molysite making to step (1), add 61.05 grams of castor oil, stir 60 minutes, then be heated to 85 ℃ of backflows 120 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, adding 3.70 concentration is the potassium hydroxide-ethanol solution of 4 mol/L, at 100 ℃, continue to stir 4 hours, then cool to room temperature, after centrifugation ethanol washs 3 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
embodiment 6:
(1) 0.50 gram of molysite mixture (mixture of 1 mM of ferric nitrate and 0.5 mM of frerrous chloride) is joined in 25 grams of ethanol, stir and it was fully dissolved in 45 minutes, make the ethanolic solution that contains molysite.
(2) in the ethanolic solution that contains molysite making to step (1), add 100 grams of castor oil, stir 90 minutes, then be heated to 95 ℃ of backflows 120 minutes, make the castor oil solution that contains molysite.
(3) in the castor oil solution that contains molysite step (2) being made, adding 5 grams of concentration is the ammonia spirit of 4 mol/L, at 120 ℃, continue to stir 3 hours, then cool to room temperature, after centrifugation ethanol washs 3 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil.
Described chemical reagent is chemical pure.
Claims (1)
1. a preparation method for the coated superparamag-netic iron oxide of castor oil, is characterized in that concrete steps are:
(1) the molysite mixture of 1 weight portion is joined in the alcohol of 10 ~ 50 weight portions, stir and it was fully dissolved in 5 ~ 120 minutes, make the alcoholic solution that contains molysite;
(2) castor oil that adds 80 ~ 200 weight portions in the alcoholic solution that contains molysite making to step (1), stirs 30 ~ 120 minutes, then is heated to 75 ~ 95 ℃ of backflows 30 ~ 120 minutes, makes the castor oil solution that contains molysite;
(3) alkaline solution that adds 5 ~ 10 weight portions in the castor oil solution that contains molysite making to step (2), at 75 ~ 180 ℃, continue to stir 0.1 ~ 5 hour, then cool to room temperature, after centrifugation ethanol washs 3 ~ 4 times, at 60 ℃, be dried 12 hours, make the coated superparamag-netic iron oxide of castor oil;
Described molysite mixture is the mixture of trivalent iron salt and divalent iron salt, and wherein the mol ratio of trivalent iron salt and divalent iron salt is 2:1, and trivalent iron salt is a kind of in iron chloride, ferric nitrate and ferric sulfate, and divalent iron salt is frerrous chloride;
Described alcohol is a kind of in ethanol, methyl alcohol, ethylene glycol, diethylene glycol (DEG) and glycerol;
Described alkaline solution be amount of substance concentration be 4 mol/L ammoniacal liquor, NaOH ethanolic solution and potassium hydroxide-ethanol solution in a kind of;
Described chemical reagent is chemical pure and above purity.
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| JP2010505736A (en) * | 2006-10-11 | 2010-02-25 | ビーエーエスエフ ソシエタス・ヨーロピア | Method for producing surface-modified nanoparticulate metal oxide, metal hydroxide and / or metal oxyhydroxide |
| CN101003386B (en) * | 2006-10-19 | 2010-05-12 | 河南大学 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
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