CN101162634A - Ion liquid based magnetofluid preparation method - Google Patents

Ion liquid based magnetofluid preparation method Download PDF

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Publication number
CN101162634A
CN101162634A CNA2007100461826A CN200710046182A CN101162634A CN 101162634 A CN101162634 A CN 101162634A CN A2007100461826 A CNA2007100461826 A CN A2007100461826A CN 200710046182 A CN200710046182 A CN 200710046182A CN 101162634 A CN101162634 A CN 101162634A
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China
Prior art keywords
room temperature
preparation
ionic liquid
tetrafluoroborate
magnetic fluid
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Pending
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CNA2007100461826A
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Chinese (zh)
Inventor
单永奎
董健媛
薛燕
杨帆
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East China Normal University
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East China Normal University
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Priority to CNA2007100461826A priority Critical patent/CN101162634A/en
Publication of CN101162634A publication Critical patent/CN101162634A/en
Pending legal-status Critical Current

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Abstract

The invention relates to room temperature ionic liquid magnetic fluid materials and a preparation method thereof, belonging to the material and the preparation thereof technical field. The invention applies the chemical coprecipitation method to prepare the nanometer-level Fe3O4 particles of which the face treatment is conducted by using the betaine as the surface active agent, and then the particles are evenly dispersed in the room temperature ion liquid, in the end the room temperature ionic liquid magnetic fluid materials are made. During the preparing process, the oxygen does not need to be excluded; the made Fe3O4 particles are small in diameter, narrowly distributed and relatively strong in magnetic performance; moreover, the method also has the advantages of simple and convenient operation and low priced and easily accessible raw materials, and is easy to be widely used.

Description

A kind of preparation method of ion liquid based magnetofluid
Technical field
The present invention relates to a kind of room temperature ionic liquid magnetic fluid materials and preparation method thereof, belong to material and preparation field thereof.
Background technology
Magnetic fluid is a kind ofly to change the intellectual material that controllable rheology is arranged with externally-applied magnetic field, and the ferromagnetism of its existing solid magnetic material has the flowability of liquid again.Developing magnetic fluid the earliest is as the aerospace seal material, is used widely in many fields such as electronics, chemical industry, machinery, the energy, metallurgy, biological medicine at present.
The type of magnetic fluid carrier fluid is selected according to sealing medium and operating mode, can be water, kerosene, silicone oil, mercury etc.The magnetic particle that mercury and metallicity are strong can well fuse and form stable magnetic fluid; Kerosene and silicone oil steam force down, can be practical under higher temperature, also can be applicable to sealing; Along with the development of Green Chemistry, water-based magnetic fluid is owing to being used widely especially in biomedicine field to environment is all friendly with human body.Ionic liquid at room temperature is the green solvent that receives much concern over more modern years, its thermal stability height, not flammable, vapour pressure is extremely low, reduced because of volatilization to the harm of environment and human body, be the greenization trend that meets very much current chemistry as the carrier fluid of magnetic fluid with ionic liquid at room temperature.
Summary of the invention
The object of the present invention is to provide a kind of novel room temperature ionic liquid magnetic fluid materials.
Another object of the present invention is to provide a kind of preparation method of easy and simple to handle, room temperature ionic liquid magnetic fluid that environmental effect is good.
Room temperature ionic liquid magnetic fluid of the present invention is made up of magnetic Nano Fe3O4, betaine coating layer and carrier ion liquid, and wherein the particle diameter of magnetic Nano Fe3O4 is 8.9-12.5nm, and saturation magnetization is 39-45emu/g.
The preparation method of above-mentioned magnetic fluid adopts chemical coprecipitation to make, and its concrete processing step is as follows:
The first step, raw material are equipped with: ferric nitrate is mixed with the aqueous solution of 0.12-0.24mol/L, ferrous sulfate is mixed with the aqueous solution of 0.08-0.16mol/L;
Second step, nanometer Fe 3O 4Preparation: get 10ml iron nitrate aqueous solution and 10ml ferrous sulfate aqueous solution, mix and stir, in 40 ℃ of waters bath with thermostatic control, add 1.6-3.2ml ammoniacal liquor (25%) fast, reaction 15min is warming up to 60 ℃, stirs 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid, the black precipitate that obtains at last is exactly a nanometer Fe 3O 4
The 3rd step, the preparation of betaine compound particle: to the Fe of washes clean 3O 4Add 30ml distilled water in the moist precipitate, ultrasonic 2min, the dark solution of the diffusing homogeneous of can getting a point.Dripping rare HCl to pH value is about 5, and 0.6-1.2ml alkali solution of beet (30%) is joined in this solution, stirs 6h, with the precipitation of acetone washing generation;
The 4th step, the preparation of magnetic fluid: get the moist precipitate after 0.5g washs with acetone, be scattered in the 10ml ionic liquid at room temperature, stir, small amount of acetone wherein can be removed ultrasonic 2min by heating a little, add 2ml polyethylene glycol-400 again, stir, ultrasonic 2min finally can get room temperature ionic liquid magnetic fluid.
The preparation method of room temperature ionic liquid magnetic fluid of the present invention, wherein the ionic liquid at room temperature in the 4th step is that 1-butyl-3-methyl imidazolium tetrafluoroborate, [EtEtIm] BF4 are that 1-ethyl-3-ethyl imidazol(e) tetrafluoroborate, [BuEtIm] BF4 are that 1-butyl-3-ethyl imidazol(e) tetrafluoroborate, [EtPy] BF4 are that N-ethylpyridine tetrafluoroborate or [BuPy] BF4 are N-butyl-pyridinium tetrafluoroborate for [BuMeIm] BF4.
Basic principle of the present invention is: utilize chemical coprecipitation to prepare nanometer Fe 3O 4, the carboxyl in the betaine can and Fe 3O 4Particle surface generation chemical bonding, and alkyl chain can stop the reunion of nano particle, surface-treated nano particle is dispersed in the ionic liquid at room temperature can obtains stable magnetic fluid.
The inventive method compared with prior art has the following advantages:
(1) the present invention adopts chemical coprecipitation to prepare Fe 3O 4, this method is easy and simple to handle, to instrument and experiment condition require low because reaction temperature is low, so do not need under the environment of anaerobic, to react.
(2) nanometer Fe that makes 3O 4Particle diameter is little, and it is all narrow to distribute, and it is stronger to have coated the saturation magnetization behind the betaine, is good magnetic material.
(3) this magnetic fluid is a carrier fluid with the ionic liquid at room temperature, is surfactant with the betaine, and is all harmless to environment and human body, meets the requirement of Green Chemistry.
(4) raw material is easy to get inexpensively, is easy to commercial Application.
Embodiment
Embodiment 1:
Get the iron nitrate solution of 10ml 0.12mol/L and the copperas solution of 10ml 0.08mol/L, mixed and stir, in 40 ℃ of waters bath with thermostatic control, add 1.6ml ammoniacal liquor (25%) fast, quicken simultaneously to stir, reaction 15min is warming up to 60 ℃ and continues reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.In this black precipitate, add 30ml water, stir, ultrasonic 2min can get the dark solution that a homogeneous disperses, dripping rare HCl to pH value is about 5, add 0.6ml alkali solution of beet (30%) again, stir 6h, force particles settling with magnet, remove wherein contained water with the acetone washing, what obtain at last is surface-treated nanometer Fe 3O 4Moist precipitate with the acetone composition.The particle diameter of this magnetic compound particles is 8.9nm, and saturation magnetization is 39emu/g.Getting this moist precipitate 0.5g and be scattered in 10ml[BuMeIm] BF4 is in 1-butyl-3-methyl imidazolium tetrafluoroborate, stirs, and ultrasonic 2min adds 2ml polyethylene glycol-400, and ultrasonic 2min can get magnetic fluid.
Embodiment 2:
Processing step is identical with embodiment 1, and just changing [EtEtIm] BF4 into as the ionic liquid of carrier is 1-ethyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 3:
Processing step is identical with embodiment 1, and just changing [BuEtIm] BF4 into as the ionic liquid of carrier is 1-butyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 4:
Processing step is identical with embodiment 1, and just changing [EtPy] BF4 into as the ionic liquid of carrier is N-ethylpyridine tetrafluoroborate.
Embodiment 5:
Processing step is identical with embodiment 1, and just changing [BuPy] BF4 into as the ionic liquid of carrier is N-butyl-pyridinium tetrafluoroborate.
Embodiment 6:
Get the iron nitrate solution of 10ml 0.18mol/L and the copperas solution of 10ml 0.12mol/L, mixed and stir, in 40 ℃ of waters bath with thermostatic control, add 2.4ml ammoniacal liquor (25%) fast, quicken simultaneously to stir, reaction 15min is warming up to 60 ℃ and continues reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.In this black precipitate, add 30ml water, stir, ultrasonic 2min can get the dark solution that a homogeneous disperses, dripping rare HCl to pH value is about 5, add 0.9ml alkali solution of beet (30%) again, stir 6h, force particles settling with magnet, remove wherein contained water with the acetone washing, what obtain at last is surface-treated nanometer Fe 3O 4Moist precipitate with the acetone composition.The particle diameter of this magnetic compound particles is 10nm, and saturation magnetization is 41emu/g.Getting this moist precipitate 0.5g and be scattered in 10ml[BuMeIm] BF4 is in 1-butyl-3-methyl imidazolium tetrafluoroborate, stirs, and ultrasonic 2min adds 2ml polyethylene glycol-400, and ultrasonic 2min can get magnetic fluid.
Embodiment 7:
Processing step is identical with embodiment 6, and just changing [EtEtIm] BF4 into as the ionic liquid of carrier is 1-ethyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 8:
Processing step is identical with embodiment 6, and just changing [BuEtIm] BF4 into as the ionic liquid of carrier is 1-butyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 9:
Processing step is identical with embodiment 6, and just changing [EtPy] BF4 into as the ionic liquid of carrier is N-ethylpyridine tetrafluoroborate.
Embodiment 10:
Processing step is identical with embodiment 6, and just changing [BuPy] BF4 into as the ionic liquid of carrier is N-butyl-pyridinium tetrafluoroborate.
Embodiment 11:
Get the iron nitrate solution of 10ml 0.24mol/L and the copperas solution of 10ml 0.16mol/L, mixed and stir, in 40 ℃ of waters bath with thermostatic control, add 3.2ml ammoniacal liquor (25%) fast, quicken simultaneously to stir, reaction 15min is warming up to 60 ℃ and continues reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.In this black precipitate, add 30ml water, stir, ultrasonic 2min can get the dark solution that a homogeneous disperses, dripping rare HCl to pH value is about 5, add 1.2ml alkali solution of beet (30%) again, stir 6h, force particles settling with magnet, remove wherein contained water with the acetone washing, what obtain at last is surface-treated nanometer Fe 3O 4Moist precipitate with the acetone composition.The particle diameter of this magnetic compound particles is 12.5nm, and saturation magnetization is 45emu/g.Getting this moist precipitate 0.5g and be scattered in 10ml[BuMeIm] BF4 is in 1-butyl-3-methyl imidazolium tetrafluoroborate, stirs, and ultrasonic 2min adds 2ml polyethylene glycol-400, and ultrasonic 2min can get magnetic fluid.
Embodiment 12:
Processing step is identical with embodiment 11, and just changing [EtEtIm] BF4 into as the ionic liquid of carrier is 1-ethyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 13:
Processing step is identical with embodiment 11, and just changing [BuEtIm] BF4 into as the ionic liquid of carrier is 1-butyl-3-ethyl imidazol(e) tetrafluoroborate.
Embodiment 14:
Processing step is identical with embodiment 11, and just changing [EtPy] BF4 into as the ionic liquid of carrier is N-ethylpyridine tetrafluoroborate.
Embodiment 15:
Processing step is identical with embodiment 11, and just changing [BuPy] BF4 into as the ionic liquid of carrier is N-butyl-pyridinium tetrafluoroborate.

Claims (3)

1. an ion liquid based magnetofluid is characterized in that by magnetic Nano Fe 3O 4, betaine coating layer and ionic liquid at room temperature carrier form, magnetic Nano Fe wherein 3O 4Particle diameter be 8.9-12.5nm, saturation magnetization is 39-45emu/g.
2. the preparation method of an ion liquid based magnetofluid adopts chemical coprecipitation, it is characterized in that comprising following step:
The first step, nanometer Fe 3O 4Preparation: getting iron nitrate aqueous solution and the 10ml concentration that 10ml concentration is 0.12-0.24mol/L is the ferrous sulfate aqueous solution of 0.08-0.16mol/L, mixing also stirs, in 40 ℃ of waters bath with thermostatic control, add 1.6-3.2ml, 25% ammoniacal liquor, reaction 15min, be warming up to 60 ℃, stir, with the black precipitate of distilled water washing generation, until supernatant liquid is neutral, and the black precipitate that obtains is exactly a nanometer Fe 3O 4
Second step, the preparation of betaine compound particle: to the Fe of washes clean 3O 4Add 30ml distilled water in the moist precipitate, ultrasonic disperse dark solution, dripping HCl to pH value is 5, with 0.6-1.2ml, 30% alkali solution of beet adds in the dark solution after disperseing, stirs, with the precipitation of acetone washing generation;
The 3rd step, the preparation of magnetic fluid: get the moist precipitate after 0.5g washs with acetone, be scattered in the 10ml ionic liquid at room temperature, stir, small amount of acetone is wherein removed by heating, ultrasonic dispersion, add 2ml polyethylene glycol-400 again, ultrasonic dispersion finally can get room temperature ionic liquid magnetic fluid.
3. the preparation method of room temperature ionic liquid magnetic fluid as claimed in claim 2 is characterized in that the ionic liquid at room temperature in the 3rd step is that 1-butyl-3-methyl imidazolium tetrafluoroborate, [EtEtIm] BF4 are that 1-ethyl-3-ethyl imidazol(e) tetrafluoroborate, [BuEtIm] BF4 are that 1-butyl-3-ethyl imidazol(e) tetrafluoroborate, [EtPy] BF4 are that N-ethylpyridine tetrafluoroborate or [BuPy] BF4 are N-butyl-pyridinium tetrafluoroborate for [BuMeIm] BF4.
CNA2007100461826A 2007-09-20 2007-09-20 Ion liquid based magnetofluid preparation method Pending CN101162634A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250868A (en) * 2010-05-21 2011-11-23 中国科学院过程工程研究所 Method for immobilizing enzyme by using magnetic ionic liquid composite material
CN102974285A (en) * 2012-12-03 2013-03-20 南京大学 Producing method of magnetic microsphere with hierarchical-pore structure and adjustable uniform grain size
DE102012016222A1 (en) 2012-08-01 2014-02-06 Technische Universität Dresden Cylinder-, piston- and valveless, continuously working fluid working machine for e.g. dosing liquid in chemical system during plastic production, has blocking region, where portions of liquids slide from region side to region opposite side
CN104030363A (en) * 2014-02-17 2014-09-10 瑞安市浙工大技术转移中心 Preparing method of ferroferric oxide nanometer particles
CN104225631A (en) * 2014-09-05 2014-12-24 中国科学院理化技术研究所 Microcapsule having function of treating tumors through magnetic resonance imaging and microwave as well as preparation method and application of microcapsule
CN107967975A (en) * 2017-12-13 2018-04-27 江西伟普科技有限公司 A kind of preparation method of the corrosion resistant environment-friendly type injection molding adhesion magnetic material of high specific gravity
CN108910961A (en) * 2018-09-03 2018-11-30 谢燕青 A kind of preparation method of ferroso-ferric oxide
CN113351109A (en) * 2021-06-04 2021-09-07 江南大学 Switch type composite emulsifier containing boric acid-based surfactant and application thereof
CN113563895A (en) * 2021-07-27 2021-10-29 华东理工大学 Heavy metal compound contaminated soil remediation agent and preparation method and application thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250868A (en) * 2010-05-21 2011-11-23 中国科学院过程工程研究所 Method for immobilizing enzyme by using magnetic ionic liquid composite material
DE102012016222A1 (en) 2012-08-01 2014-02-06 Technische Universität Dresden Cylinder-, piston- and valveless, continuously working fluid working machine for e.g. dosing liquid in chemical system during plastic production, has blocking region, where portions of liquids slide from region side to region opposite side
CN102974285A (en) * 2012-12-03 2013-03-20 南京大学 Producing method of magnetic microsphere with hierarchical-pore structure and adjustable uniform grain size
CN104030363A (en) * 2014-02-17 2014-09-10 瑞安市浙工大技术转移中心 Preparing method of ferroferric oxide nanometer particles
CN104030363B (en) * 2014-02-17 2016-05-25 瑞安市浙工大技术转移中心 A kind of preparation method of ferriferrous oxide nano-particle
CN104225631A (en) * 2014-09-05 2014-12-24 中国科学院理化技术研究所 Microcapsule having function of treating tumors through magnetic resonance imaging and microwave as well as preparation method and application of microcapsule
CN104225631B (en) * 2014-09-05 2016-08-17 中国科学院理化技术研究所 A kind of have nuclear magnetic resonance microcapsule with micro-wave therapeutic tumor function and its preparation method and application
CN107967975A (en) * 2017-12-13 2018-04-27 江西伟普科技有限公司 A kind of preparation method of the corrosion resistant environment-friendly type injection molding adhesion magnetic material of high specific gravity
CN108910961A (en) * 2018-09-03 2018-11-30 谢燕青 A kind of preparation method of ferroso-ferric oxide
CN113351109A (en) * 2021-06-04 2021-09-07 江南大学 Switch type composite emulsifier containing boric acid-based surfactant and application thereof
CN113563895A (en) * 2021-07-27 2021-10-29 华东理工大学 Heavy metal compound contaminated soil remediation agent and preparation method and application thereof
CN113563895B (en) * 2021-07-27 2022-04-01 华东理工大学 Heavy metal compound contaminated soil remediation agent and preparation method and application thereof

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