CN102360676A - Method for preparing magneto conducting magnetic fluid - Google Patents

Method for preparing magneto conducting magnetic fluid Download PDF

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Publication number
CN102360676A
CN102360676A CN2011102989734A CN201110298973A CN102360676A CN 102360676 A CN102360676 A CN 102360676A CN 2011102989734 A CN2011102989734 A CN 2011102989734A CN 201110298973 A CN201110298973 A CN 201110298973A CN 102360676 A CN102360676 A CN 102360676A
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magnetic
liquid
sulfuric acid
fe3o4
particles
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CN102360676B (en
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谢宇
黄彦
李明俊
洪小伟
余远福
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Nanchang Hangkong University
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Nanchang Hangkong University
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Abstract

The invention is aimed at providing a method for preparing magneto conducting magnetic fluid. The method comprises the following preparing processes of A. adding aniline, concentrated sulfuric acid and inhibitor in MassartFe3O4 magnetic fluid, and slowly adding water solution of ammonium persulfate during an ice-water bath; B. after reaction, performing suction filtering and washing to obtain Fe3O4/PANI compound particles; C. adding the prepared Fe3O4/PANI compound particles in the mixed solution of sodium dodecyl benzene sulfonate water solution and ethanol, stirring and reacting for 24h at room temperature; and D. centrifugally removing the Fe3O4/PANI compound particles with larger diameter by using a high-speed centrifugal machine, taking the supernate and obtaining the magneto conducting magnetic fluid. The method provided by the invention has the following advantages that the polyaniline is adopted to coat Fe3O4 magnetic particles which are about 10 nm, and the diameter of the coated compound particles is controlled, and the sodium dodecyl benzene sulfonate is induced in the coated particles and used as a dopant, repellent and hydrophilic agent, so that the novel magneto-optical material with conductive particles, adjustable dielectric constant, controllable magnetic filed can be obtained.

Description

A kind of preparation method of mangneto electricity magnetic conductivity liquid
Technical field
The present invention relates to a kind of preparation method of water-base magnetic liquid, relate in particular to and have nucleocapsid structure organic semiconductor polyaniline and coat Fe 3O 4The preparation method of the water-base magnetic liquid of magnetic nanoparticle.
Technical background
Magnetic liquid is by particle stabilized stable suspension, its nano grain surface absorption surface activating agent or the same sex electric charge generation repulsive interaction in certain base fluid of the ferromagnetic and ferrous magnetic in the 10nm left and right sides.Since strong Brownian movement, thus keep nano particle to suspend, do not take place to reunite and sedimentation.The surfactant of general magnetic liquid is through machine high score chain, does not have the potentiality of conduction, and conductive materials such as coated metal simple substance or carbon are not easy to just reunite deposition because of particle has repulsive interaction.If the magnetic nanoparticle in the magnetic liquid is coated by organic semiconductor and can stable suspersion in base fluid, then form a kind of novel magnetic liquid, be referred to as mangneto electricity magnetic conductivity liquid.Magnetic-particle produces chain or columnar microstructure in magnetic field, even cylinder system generation pseudo-crystal preface structure, and these conductive chain posts will make the conductivity of whole magnetic liquid greatly strengthen.The microstructure of chain cylinder system will exert an influence to transmitted light; And clad material is originally as organic semiconductor; Has the electrical property that is different from insulator and conductor; Can change conductivity through mixing, thereby mangneto electricity magnetic conductivity liquid has controlled dielectric property, the electric magnetic conductivity liquid of mangneto that therefore has magnetic control and dielectric adjustable will have great potential in the application in fields such as micro-optic device and photonic crystal.
But the preparation of mangneto electricity magnetic conductivity liquid need overcome two big difficulties: the one, and magnetic nanoparticle needs quilt one by one to coat; The 2nd, organic semiconductor is wanted possess hydrophilic property and mutual repellency.The present invention just is being based on and is overcoming above two difficulties, makes at Fe 3O 4Coat polyaniline on the magnetic nanoparticle and on polyaniline, introduced functional group, realized the stable suspersion of coated particle.
Summary of the invention
The object of the present invention is to provide a kind of magnetic nanoparticle surface to coat the preparation method of organic semi-conductor magnetic liquid; Its particle surface of magnetic liquid that exists at present all is that nonconducting organic long-chain molecule coats; Magnetic field control is in very big resistance states down basically, and the particle dielectric constant of coated state also is nonadjustable.The present invention uses polyaniline to coat the Fe about 10 nanometers 3O 4Magnetic-particle, and on coated particle, introduce neopelex as dopant, repellents and hydrophilizing agent, have conductivity, dielectric-constant adjustable, the controllable novel magneto-optic memory technique in magnetic field thereby obtain particle---mangneto electricity magnetic conductivity liquid.
The present invention realizes that so required preparation material is:
1. a kind of ion-type magnetic liquid is to be the Fe of 6--12nm by the fluid mechanics diameter 3O 4Magnetic-particle is formed the Massart magnetic liquid;
2. aniline;
3. sulfuric acid;
4. polymerization inhibitor;
5. Ammonium Persulfate 98.5;
6. neopelex;
7. ethanol.
Said material mol ratio is following:
Massart magnetic liquid 0.0001-0.0002;
Aniline 1-3;
Sulfuric acid 4--6;
Polymerization inhibitor 0.006-0.008;
Ammonium Persulfate 98.5 1--3;
Neopelex 3--5;
Ethanol 2--6.
Massart magnetic liquid material wherein is the mole ratio of magnetic nanoparticle in the magnetic liquid.
The preparation process is following:
A, aniline, the concentrated sulfuric acid and polymerization inhibitor are joined in the above-mentioned Massart magnetic liquid, ice-water bath 3h slowly adds the aqueous solution of ammonium persulfate in the ice bath process.
B, reaction finish the back suction filtration, and with 1mol/l sulfuric acid and acetone respectively give a baby a bath on the third day after its birth inferior after, to pH=7, get Fe with deionized water wash 3O 4/ PANI composite particles;
C, with the Fe for preparing 3O 4In the sodium dodecyl benzene sulfonate aqueous solution that/PANI composite particles joins and the mixed solution of ethanol, stirring reaction 24h under the room temperature;
D, with the larger-diameter Fe of the centrifugal removal of supercentrifuge 3O 4/ PANI composite particles is got its upper strata liquid and is promptly got mangneto electricity magnetic conductivity liquid.
Advantage of the present invention is: the Fe about the present invention uses polyaniline to 10 nanometers 3O 4Magnetic-particle coats; Adopted polymerization inhibitor,, formed the low activity free radical that the non-free radical material maybe can not cause, thereby polymerization is stopped, reduced the degree of polymerization of aniline, reached control Fe through polymerization inhibitor molecule and chain radical reaction 3O 4The effect of/polyaniline composite particles particle diameter; Adopt neopelex to increase its hydrophily as surfactant and dopant; Adopt the aqueous solution of ethanol to strengthen chemical stability as carrier fluid.Thereby obtain particle and have conductivity, dielectric-constant adjustable, the controllable novel magneto-optic memory technique in magnetic field---mangneto electricity magnetic conductivity liquid.
Embodiment
In conjunction with the foregoing invention content following case study on implementation is provided.
Embodiment 1:
A, the polymerization inhibitor of 0. 5ml aniline, the 2ml concentrated sulfuric acid and minute quantity is joined 60ml Fe 3O 4The granule fluid aerodynamic diameter is that 10nm, volume fraction are in 0.5% the Massart magnetic liquid, and ice-water bath 3h slowly adds the aqueous solution of 25ml 0.4mol/l ammonium persulfate in the ice bath process.
B, reaction finish the back suction filtration, and with 2mol/l sulfuric acid and acetone respectively give a baby a bath on the third day after its birth inferior after, to PH=7, get Fe with deionized water wash 3O 4/ PANI composite particles;
C, with the Fe for preparing 3O 4/ PANI composite particles joins in the mixed solution of sodium dodecyl benzene sulfonate aqueous solution and 50ml 0.5mol/l ethanol of 50ml 0.5mol/l, stirring reaction 24h under the room temperature;
D, with supercentrifuge 10 4Revolutions per second larger-diameter Fe of centrifugal removal 3O 4/ PANI composite particles is got its upper strata liquid and is promptly got mangneto electricity magnetic conductivity liquid.
Embodiment 2:
A, the polymerization inhibitor of 0.75ml aniline, the 2ml concentrated sulfuric acid and minute quantity is joined 50ml Fe 3O 4The granule fluid aerodynamic diameter is that 9nm, volume fraction are in 0.5% the Massart magnetic liquid, and ice-water bath 3h slowly adds the aqueous solution of 20ml 0.4mol/l ammonium persulfate in the ice bath process.
B, reaction finish the back suction filtration, and with 1mol/l sulfuric acid and acetone respectively give a baby a bath on the third day after its birth inferior after, to PH=7, get Fe with deionized water wash 3O 4/ PANI composite particles;
C, with the Fe for preparing 3O 4/ PANI composite particles joins in the mixed solution of sodium dodecyl benzene sulfonate aqueous solution and 50ml 0.5mol/l ethanol of 50ml 0.5mol/l, stirring reaction 24h under the room temperature;
D, with supercentrifuge 10 4Revolutions per second larger-diameter Fe of centrifugal removal 3O 4/ PANI composite particles is got its upper strata liquid and is promptly got mangneto electricity magnetic conductivity liquid.

Claims (2)

1. the preparation method of mangneto electricity magnetic conductivity liquid, required preparation material is:
(1), the Fe for preparing 3O 4Magnetic-particle fluid mechanics diameter is the Massart magnetic liquid of 6--12nm; Aniline; Sulfuric acid; Polymerization inhibitor; Ammonium Persulfate 98.5; Neopelex; Ethanol;
The preparation process is following:
A, aniline, the concentrated sulfuric acid and polymerization inhibitor are joined in the above-mentioned Massart magnetic liquid, ice-water bath 2-3h slowly adds the aqueous solution of ammonium persulfate in the ice bath process;
B, reaction finish the back suction filtration, and with 1mol/l sulfuric acid and acetone respectively give a baby a bath on the third day after its birth inferior after, to PH=7, get Fe with deionized water wash 3O 4/ PANI composite particles;
C, with the Fe for preparing 3O 4In the sodium dodecyl benzene sulfonate aqueous solution that/PANI composite particles joins and the mixed solution of ethanol, stirring reaction 24h under the room temperature;
D, with the larger-diameter Fe of the centrifugal removal of supercentrifuge 3O 4/ PANI composite particles is got its upper strata liquid and is promptly got mangneto electricity magnetic conductivity liquid.
2. a kind of Fe according to claim 1 3O 4The magnetic nanoparticle surface coats the preparation method of organic semi-conductor magnetic liquid, and said material mol ratio is following:
Massart magnetic liquid 0.0001-0.0002;
Aniline 1-3;
Sulfuric acid 4--6;
Polymerization inhibitor 0.006-0.008;
Ammonium Persulfate 98.5 1--3;
Neopelex 3--5;
Ethanol 2--6;
Massart magnetic liquid material wherein is the mole ratio of magnetic nanoparticle in the magnetic liquid.
CN201110298973.4A 2011-09-29 2011-09-29 Method for preparing magneto conducting magnetic fluid Expired - Fee Related CN102360676B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103617858A (en) * 2013-11-19 2014-03-05 南昌航空大学 Preparation method of magnetic fluids with polyaniline derivatives wrapping nano magnetic particles
CN103632800A (en) * 2013-12-03 2014-03-12 东华理工大学 Method for preparing polyaniline coated Fe3O4 magnetic fluid
CN103745794A (en) * 2014-01-15 2014-04-23 南昌航空大学 Step-by-step-prepared magnetic liquid with magnetic nanoparticles wrapped by polyaniline derivatives
CN107880489A (en) * 2017-11-24 2018-04-06 武汉理工大学 A kind of preparation method of anisotropic conductive epoxy resin composite material
CN111175675A (en) * 2019-12-30 2020-05-19 电子科技大学 Magnetic field sensor based on organic field effect transistor and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04118902A (en) * 1990-05-10 1992-04-20 Nok Corp Magnetic fluid whose discoloration has been prevented
CN1096487C (en) * 1999-07-12 2002-12-18 武汉工业大学 nm-class composite polyphenylamine-Fe2O3 material and its preparing process
CN101161725A (en) * 2007-09-29 2008-04-16 复旦大学 Polyaniline coated magnetic carbon-nano tube composite material and preparation method thereof
CN101280106A (en) * 2008-05-30 2008-10-08 昆明理工大学 Preparation of magnetic conductive polyaniline nanometer composite material
CN101885915A (en) * 2010-08-11 2010-11-17 哈尔滨工业大学 Method for preparing magnetic ferroferric oxide/conductive polyaniline light-weight composite hollow microspheres

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04118902A (en) * 1990-05-10 1992-04-20 Nok Corp Magnetic fluid whose discoloration has been prevented
CN1096487C (en) * 1999-07-12 2002-12-18 武汉工业大学 nm-class composite polyphenylamine-Fe2O3 material and its preparing process
CN101161725A (en) * 2007-09-29 2008-04-16 复旦大学 Polyaniline coated magnetic carbon-nano tube composite material and preparation method thereof
CN101280106A (en) * 2008-05-30 2008-10-08 昆明理工大学 Preparation of magnetic conductive polyaniline nanometer composite material
CN101885915A (en) * 2010-08-11 2010-11-17 哈尔滨工业大学 Method for preparing magnetic ferroferric oxide/conductive polyaniline light-weight composite hollow microspheres

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103617858A (en) * 2013-11-19 2014-03-05 南昌航空大学 Preparation method of magnetic fluids with polyaniline derivatives wrapping nano magnetic particles
CN103632800A (en) * 2013-12-03 2014-03-12 东华理工大学 Method for preparing polyaniline coated Fe3O4 magnetic fluid
CN103745794A (en) * 2014-01-15 2014-04-23 南昌航空大学 Step-by-step-prepared magnetic liquid with magnetic nanoparticles wrapped by polyaniline derivatives
CN103745794B (en) * 2014-01-15 2016-05-25 南昌航空大学 The magnetic liquid of polyaniline derivative parcel nano magnetic particle is prepared in a kind of substep assembling
CN107880489A (en) * 2017-11-24 2018-04-06 武汉理工大学 A kind of preparation method of anisotropic conductive epoxy resin composite material
CN111175675A (en) * 2019-12-30 2020-05-19 电子科技大学 Magnetic field sensor based on organic field effect transistor and preparation method thereof

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