CN107969437A - The preparation method of ferroso-ferric oxide silver-carrying nano particle - Google Patents
The preparation method of ferroso-ferric oxide silver-carrying nano particle Download PDFInfo
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- CN107969437A CN107969437A CN201711295919.8A CN201711295919A CN107969437A CN 107969437 A CN107969437 A CN 107969437A CN 201711295919 A CN201711295919 A CN 201711295919A CN 107969437 A CN107969437 A CN 107969437A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
Abstract
The present invention discloses a kind of preparation method of ferroso-ferric oxide silver-carrying nano particle, comprises the following steps：（1）Silver acetate and oleyl amine are mixed, reacts under nitrogen atmosphere, obtains silver acetate oleyl amine mixed liquor；（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, stirring, ultrasonic disperse, washing, then by the organic phase rotary evaporation of generation, obtains iron oleate；（3）Iron oleate is dissolved in 1 octadecylene, is reacted under nitrogen atmosphere, reaction product adds in ethanol and obtains sediment, and sediment magnetic is separated, is washed 3 times with n-hexane, ethanol respectively, obtains ferriferrous oxide nano magnetic particle；（4）Into the hexane solution of ferriferrous oxide nano magnetic particle, silver acetate oleyl amine mixed liquor is added dropwise, under nitrogen atmosphere, stirring, then by product Magneto separate, is washed with ethanol, obtain ferroso-ferric oxide silver-carrying nano particle.This method is easy to operate, and product size is homogeneous, good anti-bacterial effect.
Description
Technical field
The invention belongs to anti-biotic material technical field, and in particular to a kind of preparation side of ferroso-ferric oxide silver-carrying nano particle
Method.
Background technology
In recent years, the application potential of super paramagnetic material causes the extensive research interest of researcher, such as magnetic resonance
Contrast-enhancing agent in imaging, the sequence of magnetic auxiliary cell and separation etc..Wherein, nano ferriferrous oxide has the excellent of nano material concurrently
Different physicochemical properties and magnetic property, have the characteristics such as superparamagnetic, good biocompatibility, it is a kind of excellent as magnetic carrier
Selection.Before this, the synthetic method to ferriferrous oxide nano-particle and pattern control research it is extensive, it has been reported that have solvent
Hot method, chemical coprecipitation and high-temperature cracking method etc..Moreover, silver and silver composite have potent resist as a kind of antiseptic
The performance of bacterium ability and broad suppression microbe species.By the compounding design of nano-particle, on nano ferriferrous oxide
It is brilliant to grow silver nanoparticle, prepares and both possesses excellent antibacterial characteristics, can also realize the manipulation of targeting material with it is separated new
Multifunctional material.
At present, the research of different types of magnetic silver-carrying nano particle has been seen in report, there is research Nano silver grain combination hydrogen
Key multi-layer polyelectrolyte film is assembled in magnetic carrier；Also research prepares ferroso-ferric oxide with coprecipitation, then in microemulsion
Reduction silver nitrate prepares magnetic silver-carrying nano material.Lan Yanna etc. is prepared for ferroso-ferric oxide using coprecipitation, is given birth to using crystal seed
Regular way further prepares magnetic silver-carrying nano material.Solemnity etc. prepares magnetic nano-particle using chemical coprecipitation, then with 3- mercaptos
Base propyl trimethoxy silicane is modified, and connection Nano silver grain prepares core shell structure magnetic silver-carrying nano material.But in gentle bar
In organic solvent under part, fabricated in situ silver nanoparticle is brilliant directly on magnetic nano-particle surface, and the magnetic for obtaining special pattern carries
The Nano silver grain and synthetic method for keeping its magnetic property not reduce is complicated, yield is low.
The content of the invention
The defects of for the prior art, the present invention provide a kind of preparation method of ferroso-ferric oxide silver-carrying nano particle.
The preparation method of ferroso-ferric oxide silver-carrying nano particle, comprises the following steps：
（1）The preparation of silver acetate-oleyl amine mixed liquor：By silver acetate and oleyl amine according to solid-liquid ratio 1:20 mixing, under nitrogen atmosphere
2-4h is reacted, obtains silver acetate-oleyl amine mixed liquor；
（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, the stirring reaction 2-3h at 70-85 DEG C, so
Ultrasonic disperse 15min afterwards, is washed with distilled water 3 times, then by the organic phase rotary evaporation of generation, obtains iron oleate；
（3）Iron oleate is dissolved in 1- octadecylenes, under nitrogen atmosphere, reacts 30min at 300-350 DEG C, by reaction product plus
Enter and sediment is obtained in ethanol, sediment magnetic is separated, washed 3 times with n-hexane, ethanol respectively, obtain ferroso-ferric oxide and receive
Rice magnetic particle；
（4）Into the hexane solution of ferriferrous oxide nano magnetic particle, silver acetate-oleyl amine mixed liquor is added dropwise, in blanket of nitrogen
Under enclosing, reaction 1-2h is stirred under the rotating speed of 3000rpm, at 70 DEG C, cooled to room temperature, then by product Magneto separate, is used
Ethanol washs 3 times, obtains ferroso-ferric oxide silver-carrying nano particle.
Preferably, step（2）Middle enuatrol, ferric trichloride, ethanol, the adding proportion of n-hexane and deionized water are 10g:
7g:15mL:6mL:20mL。
Preferably, step（2）The condition of middle ultrasonic disperse is：Ultrasonic power 200-500W, supersonic frequency 40Hz.
Preferably, step（2）The condition of middle rotary evaporation is：50-60 DEG C of temperature, time 30-50min.
Preferably, step（3）The mass ratio of middle iron oleate and 1- octadecylene is 1:5.
Preferably, step（4）The mass concentration of the hexane solution of middle ferriferrous oxide nano magnetic particle is 1mg/mL.
Preferably, step（4）Hexane solution and silver acetate-oleyl amine mixed liquor of middle ferriferrous oxide nano magnetic particle
Volume ratio be 40:3.
Advantages of the present invention：
The preparation method of ferroso-ferric oxide silver-carrying nano particle provided by the invention is easy to operate, and product size is homogeneous, antibacterial effect
Fruit is good.
Embodiment
Embodiment 1
The preparation method of ferroso-ferric oxide silver-carrying nano particle, comprises the following steps：
（1）The preparation of silver acetate-oleyl amine mixed liquor：By silver acetate and oleyl amine according to solid-liquid ratio 1:20 mixing, under nitrogen atmosphere
2-4h is reacted, obtains silver acetate-oleyl amine mixed liquor；
（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, the stirring reaction 2-3h at 70-85 DEG C, so
The ultrasonic disperse 15min under conditions of ultrasonic power 200-500W, supersonic frequency 40Hz afterwards, is washed with distilled water 3 times, then will
Organic phase rotary evaporation 30-50min under conditions of 50-60 DEG C of temperature is generated, obtains iron oleate；Wherein, enuatrol, tri-chlorination
Iron, ethanol, the adding proportion of n-hexane and deionized water are 10g:7g:15mL:6mL:20mL；
（3）According to mass ratio 1:5 are dissolved in iron oleate in 1- octadecylenes, under nitrogen atmosphere, react 30min at 300-350 DEG C,
Reaction product is added in ethanol and obtains sediment, sediment magnetic is separated, is washed 3 times, obtained with n-hexane, ethanol respectively
Ferriferrous oxide nano magnetic particle；
（4）Into the hexane solution for the ferriferrous oxide nano magnetic particle that mass concentration is 1mg/mL, silver acetate-oil is added dropwise
Amine mixed liquor, wherein, the volume ratio of hexane solution and silver acetate-oleyl amine mixed liquor of ferriferrous oxide nano magnetic particle is
40:3, under nitrogen atmosphere, reaction 1-2h is stirred under the rotating speed of 3000rpm, at 70 DEG C, cooled to room temperature, then will
Product Magneto separate, is washed 3 times with ethanol, obtains ferroso-ferric oxide silver-carrying nano particle.
Embodiment 2
The preparation method of ferroso-ferric oxide silver-carrying nano particle, comprises the following steps：
（1）The preparation of silver acetate-oleyl amine mixed liquor：By silver acetate and oleyl amine according to solid-liquid ratio 1:20 mixing, under nitrogen atmosphere
2-4h is reacted, obtains silver acetate-oleyl amine mixed liquor；
（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, the stirring reaction 2-3h at 70-85 DEG C, so
The ultrasonic disperse 15min under conditions of ultrasonic power 200-500W, supersonic frequency 40Hz afterwards, is washed with distilled water 3 times, then will
Organic phase rotary evaporation 30-50min under conditions of 50-60 DEG C of temperature is generated, obtains iron oleate；Wherein, enuatrol, tri-chlorination
Iron, ethanol, the adding proportion of n-hexane and deionized water are 10g:7g:15mL:6mL:20mL；
（3）According to mass ratio 1:5 are dissolved in iron oleate in 1- octadecylenes, under nitrogen atmosphere, react 30min at 300-350 DEG C,
Reaction product is added in ethanol and obtains sediment, sediment magnetic is separated, is washed 3 times, obtained with n-hexane, ethanol respectively
Ferriferrous oxide nano magnetic particle；
（4）Into the hexane solution for the ferriferrous oxide nano magnetic particle that mass concentration is 1mg/mL, silver acetate-oil is added dropwise
Amine mixed liquor, wherein, the volume ratio of hexane solution and silver acetate-oleyl amine mixed liquor of ferriferrous oxide nano magnetic particle is
40:3, under nitrogen atmosphere, reaction 1-2h is stirred under the rotating speed of 3000rpm, at 70 DEG C, cooled to room temperature, then will
Product Magneto separate, is washed 3 times with ethanol, obtains ferroso-ferric oxide silver-carrying nano particle.
Embodiment 3
The preparation method of ferroso-ferric oxide silver-carrying nano particle, comprises the following steps：
（1）The preparation of silver acetate-oleyl amine mixed liquor：By silver acetate and oleyl amine according to solid-liquid ratio 1:20 mixing, under nitrogen atmosphere
2-4h is reacted, obtains silver acetate-oleyl amine mixed liquor；
（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, the stirring reaction 2-3h at 70-85 DEG C, so
The ultrasonic disperse 15min under conditions of ultrasonic power 200-500W, supersonic frequency 40Hz afterwards, is washed with distilled water 3 times, then will
Organic phase rotary evaporation 30-50min under conditions of 50-60 DEG C of temperature is generated, obtains iron oleate；Wherein, enuatrol, tri-chlorination
Iron, ethanol, the adding proportion of n-hexane and deionized water are 10g:7g:15mL:6mL:20mL；
（3）According to mass ratio 1:5 are dissolved in iron oleate in 1- octadecylenes, under nitrogen atmosphere, react 30min at 300-350 DEG C,
Reaction product is added in ethanol and obtains sediment, sediment magnetic is separated, is washed 3 times, obtained with n-hexane, ethanol respectively
Ferriferrous oxide nano magnetic particle；
（4）Into the hexane solution for the ferriferrous oxide nano magnetic particle that mass concentration is 1mg/mL, silver acetate-oil is added dropwise
Amine mixed liquor, wherein, the volume ratio of hexane solution and silver acetate-oleyl amine mixed liquor of ferriferrous oxide nano magnetic particle is
40:3, under nitrogen atmosphere, reaction 1-2h is stirred under the rotating speed of 3000rpm, at 70 DEG C, cooled to room temperature, then will
Product Magneto separate, is washed 3 times with ethanol, obtains ferroso-ferric oxide silver-carrying nano particle.
Claims (7)
1. the preparation method of ferroso-ferric oxide silver-carrying nano particle, it is characterised in that：Comprise the following steps：
（1）The preparation of silver acetate-oleyl amine mixed liquor：By silver acetate and oleyl amine according to solid-liquid ratio 1:20 mixing, under nitrogen atmosphere
2-4h is reacted, obtains silver acetate-oleyl amine mixed liquor；
（2）Enuatrol, ferric trichloride, ethanol, n-hexane and deionized water are mixed, the stirring reaction 2-3h at 70-85 DEG C, so
Ultrasonic disperse 15min afterwards, is washed with distilled water 3 times, then by the organic phase rotary evaporation of generation, obtains iron oleate；
（3）Iron oleate is dissolved in 1- octadecylenes, under nitrogen atmosphere, reacts 30min at 300-350 DEG C, by reaction product plus
Enter and sediment is obtained in ethanol, sediment magnetic is separated, washed 3 times with n-hexane, ethanol respectively, obtain ferroso-ferric oxide and receive
Rice magnetic particle；
（4）Into the hexane solution of ferriferrous oxide nano magnetic particle, silver acetate-oleyl amine mixed liquor is added dropwise, in blanket of nitrogen
Under enclosing, reaction 1-2h is stirred under the rotating speed of 3000rpm, at 70 DEG C, cooled to room temperature, then by product Magneto separate, is used
Ethanol washs 3 times, obtains ferroso-ferric oxide silver-carrying nano particle.
2. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（2）
Middle enuatrol, ferric trichloride, ethanol, the adding proportion of n-hexane and deionized water are 10g:7g:15mL:6mL:20mL.
3. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（2）
The condition of middle ultrasonic disperse is：Ultrasonic power 200-500W, supersonic frequency 40Hz.
4. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（2）
The condition of middle rotary evaporation is：50-60 DEG C of temperature, time 30-50min.
5. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（3）
The mass ratio of middle iron oleate and 1- octadecylene is 1:5.
6. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（4）
The mass concentration of the hexane solution of middle ferriferrous oxide nano magnetic particle is 1mg/mL.
7. the preparation method of ferroso-ferric oxide silver-carrying nano particle according to claim 1, it is characterised in that：Step（4）
The volume ratio of hexane solution and silver acetate-oleyl amine mixed liquor of middle ferriferrous oxide nano magnetic particle is 40:3.
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| CN109888154A (en) * | 2019-03-14 | 2019-06-14 | 复旦大学 | A kind of preparation method of high-performance modified polypropylene diaphragm |
| CN110261614A (en) * | 2019-06-24 | 2019-09-20 | 邓胜明 | A kind of method and application of radioiodination targeting bimetal nano material |
| CN112408495A (en) * | 2020-11-24 | 2021-02-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of superparamagnetic Ag/ferroferric oxide nanospheres |
| CN114570937A (en) * | 2022-03-04 | 2022-06-03 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
| CN116395747A (en) * | 2023-02-22 | 2023-07-07 | 浙江理工大学 | Manganese tetraoxide-silver sulfide Janus structure nanocomposite and preparation method thereof |
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2017
- 2017-12-08 CN CN201711295919.8A patent/CN107969437A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888154A (en) * | 2019-03-14 | 2019-06-14 | 复旦大学 | A kind of preparation method of high-performance modified polypropylene diaphragm |
| CN110261614A (en) * | 2019-06-24 | 2019-09-20 | 邓胜明 | A kind of method and application of radioiodination targeting bimetal nano material |
| CN112408495A (en) * | 2020-11-24 | 2021-02-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of superparamagnetic Ag/ferroferric oxide nanospheres |
| CN114570937A (en) * | 2022-03-04 | 2022-06-03 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
| CN114570937B (en) * | 2022-03-04 | 2024-03-29 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
| CN116395747A (en) * | 2023-02-22 | 2023-07-07 | 浙江理工大学 | Manganese tetraoxide-silver sulfide Janus structure nanocomposite and preparation method thereof |
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Application publication date: 20180501 |