CN109686526A - Stable magnetic fluid and preparation method thereof under the conditions of a kind of high-intensity magnetic field - Google Patents
Stable magnetic fluid and preparation method thereof under the conditions of a kind of high-intensity magnetic field Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
The present invention provides magnetic fluid and preparation method thereof stable under the conditions of a kind of high-intensity magnetic field, preparation method includes urea liquid being added dropwise into acetylacetone,2,4-pentanedione ferrous solution, then be stirred to react, and obtains reaction solution 1；Stabiliser solution is added into reaction solution 1 under agitation, then is stirred to react, obtains reaction solution 2；Reaction solution 2 is heated, is centrifuged and washed, the magnetic powder of metatitanic acid coupling agent cladding is obtained；Ultrasonic disperse will be carried out after magnetic powder, carrier fluid and dispersant, obtains stablizing magnetic fluid.The magnetic saturation intensity for the magnetic fluid being prepared is 100~500GS；In 300KJ/m3The coefficient of stability of magnetic fluid under magnet is unchanged in six months, and magnetic fluid is good in high-intensity magnetic field stability inferior.
Description
Technical field
The present invention relates to magnetic Nano material, in particular to stable magnetic fluid and its preparation under the conditions of a kind of high-intensity magnetic field
Method.
Background technique
Magnetic fluid is a kind of novel functional material, it had not only had the mobility of liquid but also had had solid magnetic material
Magnetism is magnetic retention particle, base load liquid (being also media) and interfacial agent the three mixing by diameter for nanometer scale
Made of a kind of stable colloidal liquid.Magnetic fluid nonmagnetic attraction in static state is just showed when externally-applied magnetic field effect
It is magnetic out.It is had excellent performance with the magnetic fluid that nano metal and alloy powder produce, can be widely applied to the magnetic of various harsh conditions
Property Fluid Sealing, damping, medical instrument, sound is adjusted, light is shown, the fields such as magnetic fluid ore dressing.
Magnetofluid making method mainly has polishing, dispergation method, thermal decomposition method, electric discharge etc..It is using most at present
The magnetic ferrites materials for using coprecipitation to prepare are used as fine flour activating agent, water and lubrication as nano particle, oleic acid oleyl amine etc.
Oily (mineral oil and synthetic oil) prepares magnetic fluid as carrier.Chinese patent CN1278946A disclose a kind of magnetic fluid and its
Manufacturing method, wherein being prepared for the magnetic metal ion of 10 rans with CVD method, it is aoxidized in order to prevent, is wrapped on its surface
The oxidation-resistant film (silica) for having covered 0.01-1nm, prepares the stable magnetic fluid of performance.Chinese patent CN1774774A
A kind of magnetic fluid of chemical stability and preparation method thereof with improvement is disclosed, wherein with metal, metal alloy, metal
Mixture is nonmetallic as element modifier, and discovery plays the role of raising magnetic fluid chemical stability very big.It is Chinese special
Sharp CN1797624A discloses a kind of Ferrimagnetism fluid, wherein with divalent iron salt and trivalent iron salt in ammonium hydroxide under conditions of system
For using ferrite as the magnetic fluid of magnetic-particle.United States Patent (USP) 5676877 discloses a kind of good magnetic of chemical stability
Property fluid preparation method, wherein being prepared after completely covering magnetic nanoparticle with surface modifier (alkylol SiClx alkane)
The good magnetic fluid of chemical stabilization.
The application of magnetic fluid is all applied under strong magnetic field circumstance substantially, although the preparation method in above-mentioned patent
The chemical stability of magnetic fluid is improved to a certain degree, but it still needs further improvement for the magnetic field stability of fluid.Therefore having must
A kind of magnetic fluid that can be used steadily in the long term under the conditions of the high-intensity magnetic fields such as neodymium iron boron is provided.
Summary of the invention
The present invention provides magnetic fluids and preparation method thereof stable under the conditions of a kind of high-intensity magnetic field, and its purpose is to increase
The stability of ferromagnetism fluid can simultaneously use for a long time in high-intensity magnetic field.
In order to achieve the above object, the invention provides the following technical scheme:
The preparation method of stable magnetic fluid, includes the following steps: under the conditions of a kind of high-intensity magnetic field
1) urea liquid is added dropwise into acetylacetone,2,4-pentanedione ferrous solution, then is stirred to react, obtains reaction solution 1；
Wherein, the molar ratio of ferric acetyl acetonade and urea is 1:(1.0~5.5)；
2) stabiliser solution is added into reaction solution 1 obtained by step 1) under agitation, then is stirred to react, obtain
Reaction solution 2；
Wherein, stabilizer is metatitanic acid coupling agent, and the volume ratio of stabiliser solution and reaction solution 1 is (0.1~1): 100；
3) reaction solution 2 obtained by step 2) is heated, is centrifuged and washed, obtain the magnetic powder of metatitanic acid coupling agent cladding；
4) by magnetic powder obtained by step 3) and carrier fluid and dispersant, then ultrasonic disperse is carried out, obtains stablizing magnetic flow
Body.
Preferably, the acetylacetone,2,4-pentanedione ferrous solution is that ferric acetyl acetonade dissolution is made in ethanol, the acetylacetone,2,4-pentanedione
The mass fraction of iron is 1~20%.
Preferably, the urea liquid is that urea dissolution is made in ethanol, the mass fraction of the urea is 1~
30%.
Preferably, the stabiliser solution is that stabilizer dissolution is made in ethanol, the mass fraction of the stabilizer
It is 0.5~5%.
Preferably, described in step 1) into acetylacetone,2,4-pentanedione ferrous solution be added dropwise urea liquid be specially with 100~200 drop/
Urea liquid is added dropwise in the acetylacetone,2,4-pentanedione ferrous solution that the rate of addition of min is 40~60 DEG C to temperature.
Preferably, the step 3) heating is specially that 240~480min is reacted under the conditions of 150~200 DEG C.
Preferably, the partial size of the magnetic powder of step 3) the metatitanic acid coupling agent cladding is 5~20nm.
Preferably, the molar ratio of the step 3) magnetic powder, carrier fluid and dispersing agent is (0.1~1): 1:0.1.
Preferably, carrier fluid described in step 3) is decanedioic acid oleate, glycerol trioleate, Monoolein, laurel
One of sour oleyl alcohol ester, tricarboxymethyl propane oleate and oleyl alcohol oleate are a variety of；The dispersing agent is castor oil polyoxy
Vinethene, heterogeneous ten alcohol polyoxyethylene ether, octyl phenol polyoxyethylene ether, polyoxyethylene laurate, glycerin polyoxyethylene ether and
One of octadecylamine polyoxyethylene ether is a variety of.
The present invention also provides magnetic stable under the conditions of a kind of high-intensity magnetic field being prepared by above-mentioned any one the method
Property fluid, the magnetic saturation intensity of the magnetic fluid is 100~500GS.
Preparation provided by the invention is raw material using Organic Iron (ferric acetyl acetonade), and alkalescent urea is oxidant,
OH is discharged under certain temperature-Root obtains the Fe of size uniformity3O4Nano particle；Titanate coupling agent is used under high-temperature and high-pressure conditions
Fe is coated as surface modification stabilizer3O4Nano particle makes it have good compatibility with dispersion liquid and improve high-intensity magnetic field
Under the conditions of stability.
Above scheme of the invention have it is following the utility model has the advantages that
Preparation method provided by the invention is easy to operate, raw material is easy to get, low in cost, is suitble to large-scale production.
Fe in preparation method provided by the invention3+With OH-Reaction generates Fe3O4, Fe3O4Uniform particle diameter is conducive to the short time
Interior dispersion acts in a liquid, and the magnetic powder that can be used as in magnetic fluid uses；Make the Fe of titanate esters modification prepared by the present invention3O4
Mass fraction be 10~50%, the magnetic powder partial size of metatitanic acid coupling agent prepared by the present invention cladding is 5nm~20nm, is had good
Crystallinity and dispersibility.Fe3O4It is reacted again with stabilizer (metatitanic acid coupling agent), high-intensity magnetic field item is prepared into carrier fluid for redisperse
Stablize magnetic fluid under part；Stabilizer (metatitanic acid coupling agent), which not only plays, makes Fe3O4Stable effect, and also help magnetism
Fluid is used for a long time under the conditions of high-intensity magnetic field.
The magnetic saturation intensity for the magnetic fluid that the present invention is prepared is 100~500GS；In 300KJ/m3Magnetic under magnet
The coefficient of stability of property fluid is unchanged in six months, and magnetic fluid is good in high-intensity magnetic field stability inferior.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the magnetic powder of metatitanic acid coupling agent cladding in the embodiment of the present invention 1.
Fig. 2 is coefficient of stability figure of magnetic fluid under the conditions of high-intensity magnetic field in the embodiment of the present invention 1.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
Embodiment 1
(1) ferric acetyl acetonade is dissolved into ethyl alcohol, obtains the acetylacetone,2,4-pentanedione ferrous solution that mass fraction is 10%；
(2) urea is dissolved into ethyl alcohol, obtains the urea liquid that mass fraction is 20%；
(3) stabilizer is distributed in alcoholic solution, obtains the stabiliser solution that mass fraction is 2%；Wherein, stabilizer is
Metatitanic acid coupling agent (butyl titanate)；
(4) acetylacetone,2,4-pentanedione ferrous solution obtained by step (1) is heated to 40 DEG C, then with 100 drops/min rate of addition to temperature
Degree obtains reaction solution 1 for the urea liquid that mass fraction is 20% is added dropwise in 40 DEG C of acetylacetone,2,4-pentanedione ferrous solution；Wherein, it reacts
The molar ratio of ferric acetyl acetonade and urea is 1:1 in liquid 1；
(5) reaction solution 1 is stirred to react 10min under conditions of temperature is 40 DEG C and mixing speed is 50r/min, then
Under conditions of mixing speed is 50r/min, then stabiliser solution is added into reaction solution 1, then for 30 DEG C and is stirred fast in temperature
Degree is to be stirred to react 10min under 300r/min, obtains reaction solution 2；
Wherein, the volume ratio of the stabiliser solution and reaction solution 1 is 1:100；
(6) 2 solution of reaction solution is transferred in hydrothermal reaction kettle, reacts 240min under the conditions of 150 DEG C, obtains reaction solution
3；
(7) reaction solution 3 is cooled to room temperature, 5min is centrifuged under the conditions of centrifugal speed is 3000r/min, by reaction solution 3
Supernatant liquor pour out, reject, collect lower layer's solid matter；The ethyl alcohol for the use of temperature being 50 DEG C is to lower layer's solid matter of collection
Cleaning 3 times obtains the magnetic powder of metatitanic acid coupling agent cladding；Wherein, the magnetic powder partial size of metatitanic acid coupling agent cladding is 8nm.
(8) magnetic powder, carrier fluid (decanedioic acid oleate) and the dispersing agent (castor oil polyoxyethylene coated metatitanic acid coupling agent
Ether) be 50 DEG C in temperature at ultrasonic disperse 2h, obtain stablizing magnetic fluid under the conditions of high-intensity magnetic field；Wherein, the magnetic powder, decanedioic acid
Oleate and castor oil polyoxyethylene ether molar ratio are 1:1:0.1；The magnetic saturation intensity of the magnetic fluid is 300GS.
The transmission electron microscope picture for the magnetic powder that metatitanic acid coupling agent coats in embodiment 1 is as shown in Figure 1, the metatitanic acid coupling agent packet prepared
The Fe covered3O4Magnetic powder is spherical shape, and size is conducive to be dispersed in carrier fluid substantially in 8 rans.
Strong magnet (magnetic energy product 300KJ/m is placed on by the magnetic fluid of preparation is static3) above, routine test density, first
Density of test, the density of test in second month every ten days monthly test a density in latter 120 days, under daily within a month
Column formula calculates its coefficient of stability:
I=(ρ1-ρ)/(ρ-ρw)
Wherein I is the coefficient of stability, the magnetic fluid density of ρ test for the first time, ρ1Be it is static after the density tested every time, ρw
For the density of carrier fluid.
It is found to be the coefficient of stability by test in 180 days not change, as shown in Fig. 2, it will thus be seen that the magnetic of preparation
Property fluid it is steady in a long-term under the conditions of strong magnetic.
Embodiment 2
(1) ferric acetyl acetonade is dissolved into ethyl alcohol, obtains the acetylacetone,2,4-pentanedione ferrous solution that mass fraction is 1%；
(2) urea is dissolved into ethyl alcohol, obtains the urea liquid that mass fraction is 1%；
(3) stabilizer is distributed in alcoholic solution, obtains the stabiliser solution that mass fraction is 0.5%；Wherein, stabilizer
For metatitanic acid coupling agent (butyl titanate)；
(4) acetylacetone,2,4-pentanedione ferrous solution obtained by step (1) is heated to 50 DEG C, then with 150 drops/min rate of addition to temperature
Degree obtains reaction solution 1 for the urea liquid that mass fraction is 1% is added dropwise in 50 DEG C of acetylacetone,2,4-pentanedione ferrous solution；Wherein, reaction solution
The molar ratio of ferric acetyl acetonade and urea is 1:3 in 1；
(5) reaction solution 1 is stirred to react 20min under conditions of temperature is 50 DEG C and mixing speed is 100r/min, then
Under conditions of low whipping speed is 100r/min, then stabiliser solution is added into reaction solution 1, then for 40 DEG C and is stirred in temperature
Speed is to be stirred to react 30min under 400r/min, obtains reaction solution 2；
Wherein, the volume ratio of the stabiliser solution and reaction solution 1 is 0.5:100；
(6) 2 solution of reaction solution is transferred in hydrothermal reaction kettle, reacts 300min under the conditions of 180 DEG C, obtains reaction solution
3；
(7) reaction solution 3 is cooled to room temperature, 8min is centrifuged under the conditions of centrifugal speed is 4000r/min, by reaction solution 3
Supernatant liquor pour out, reject, collect lower layer's solid matter；The ethyl alcohol for the use of temperature being 55 DEG C is to lower layer's solid matter of collection
Cleaning 5 times obtains the magnetic powder of metatitanic acid coupling agent cladding；Wherein, the magnetic powder partial size of metatitanic acid coupling agent cladding is 5nm.
(8) magnetic powder, carrier fluid (decanedioic acid oleate) and the dispersing agent (castor oil polyoxyethylene coated metatitanic acid coupling agent
Ether) be 80 DEG C in temperature at ultrasonic disperse 3h, obtain stablizing magnetic fluid under the conditions of high-intensity magnetic field；Wherein, the magnetic powder, decanedioic acid
Oleate and castor oil polyoxyethylene ether molar ratio are 0.5:1:0.1；The magnetic saturation intensity of the magnetic fluid is 100GS.
Embodiment 3
(1) ferric acetyl acetonade is dissolved into ethyl alcohol, obtains the acetylacetone,2,4-pentanedione ferrous solution that mass fraction is 20%；
(2) urea is dissolved into ethyl alcohol, obtains the urea liquid that mass fraction is 30%；
(3) stabilizer is distributed in alcoholic solution, obtains the stabiliser solution that mass fraction is 5%；Wherein, stabilizer is
Metatitanic acid coupling agent (butyl titanate)；
(4) acetylacetone,2,4-pentanedione ferrous solution obtained by step (1) is heated to 60 DEG C, then with 200 drops/min rate of addition to temperature
Degree obtains reaction solution 1 for the urea liquid that mass fraction is 30% is added dropwise in 60 DEG C of acetylacetone,2,4-pentanedione ferrous solution；Wherein, it reacts
The molar ratio of ferric acetyl acetonade and urea is 1:5.5 in liquid 1；
(5) reaction solution 1 is stirred to react 30min under conditions of temperature is 60 DEG C and mixing speed is 200r/min, then
Under conditions of low whipping speed is 200r/min, then stabiliser solution is added into reaction solution 1, then for 50 DEG C and is stirred in temperature
Speed is to be stirred to react 60min under 800r/min, obtains reaction solution 2；
Wherein, the volume ratio of the stabiliser solution and reaction solution 1 is 1:100；
(6) 2 solution of reaction solution is transferred in hydrothermal reaction kettle, reacts 480min under the conditions of 200 DEG C, obtains reaction solution
3；
(7) reaction solution 3 is cooled to room temperature, 10min is centrifuged under the conditions of centrifugal speed is 5000r/min, by reaction solution 3
Supernatant liquor pour out, reject, collect lower layer's solid matter；The ethyl alcohol for the use of temperature being 60 DEG C is to lower layer's solid matter of collection
Cleaning 4 times obtains the magnetic powder of metatitanic acid coupling agent cladding；Wherein, the magnetic powder partial size of metatitanic acid coupling agent cladding is 20nm.
(8) magnetic powder, carrier fluid (decanedioic acid oleate) and the dispersing agent (castor oil polyoxyethylene coated metatitanic acid coupling agent
Ether) be 100 DEG C in temperature at ultrasonic disperse 5h, obtain stablizing magnetic fluid under the conditions of high-intensity magnetic field；Wherein, the magnetic powder, the last of the ten Heavenly stems two
Pinolenic acid ester and castor oil polyoxyethylene ether molar ratio are 0.1:1:0.1；The magnetic saturation intensity of the magnetic fluid is 500GS.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. the preparation method of stable magnetic fluid under the conditions of a kind of high-intensity magnetic field, which comprises the steps of:
1) urea liquid is added dropwise into acetylacetone,2,4-pentanedione ferrous solution, then is stirred to react, obtains reaction solution 1；
Wherein, the molar ratio of ferric acetyl acetonade and urea is 1:(1.0~5.5)；
2) stabiliser solution is added into reaction solution 1 obtained by step 1) under agitation, then is stirred to react, reacted
Liquid 2；
Wherein, stabilizer is metatitanic acid coupling agent, and the volume ratio of stabiliser solution and reaction solution 1 is (0.1~1): 100；
3) reaction solution 2 obtained by step 2) is heated, is centrifuged and washed, obtain the magnetic powder of metatitanic acid coupling agent cladding；
4) by magnetic powder obtained by step 3) and carrier fluid and dispersant, then ultrasonic disperse is carried out, obtains stablizing magnetic fluid.
2. preparation method according to claim 1, which is characterized in that the acetylacetone,2,4-pentanedione ferrous solution is that ferric acetyl acetonade is molten
Solution is made in ethanol, and the mass fraction of the ferric acetyl acetonade is 1~20%.
3. preparation method according to claim 1, which is characterized in that the urea liquid is to make urea dissolution in ethanol
, the mass fraction of the urea is 1~30%.
4. preparation method according to claim 1, which is characterized in that the stabiliser solution is that stabilizer is dissolved in ethyl alcohol
In be made, the mass fraction of the stabilizer is 0.5~5%.
5. preparation method according to claim 1, which is characterized in that be added dropwise described in step 1) into acetylacetone,2,4-pentanedione ferrous solution
It is dripped in the acetylacetone,2,4-pentanedione ferrous solution that urea liquid is specially 40~60 DEG C to temperature with 100~200 drops/min rate of addition
Add urea liquid.
6. preparation method according to claim 1, which is characterized in that the step 3) heating is specially in 150~200 DEG C of items
240~480min is reacted under part.
7. preparation method according to claim 1, which is characterized in that the grain of the magnetic powder of step 3) the metatitanic acid coupling agent cladding
Diameter is 5~20nm.
8. preparation method according to claim 1, which is characterized in that mole of the step 3) magnetic powder, carrier fluid and dispersing agent
Than for (0.1~1): 1:0.1.
9. preparation method according to claim 1, which is characterized in that carrier fluid described in step 3) is decanedioic acid oleate, sweet
One of oily trioleate, Monoolein, lauric acid oil alcohol ester, tricarboxymethyl propane oleate and oleyl alcohol oleate or
It is a variety of；The dispersing agent is castor oil polyoxyethylene ether, heterogeneous ten alcohol polyoxyethylene ether, octyl phenol polyoxyethylene ether, polyoxy second
One of alkene laurate, glycerin polyoxyethylene ether and octadecylamine polyoxyethylene ether are a variety of.
10. stable magnetic fluid under the conditions of a kind of high-intensity magnetic field being prepared by claim 1-9 any one the method,
It is characterized in that, the magnetic saturation intensity of the magnetic fluid is 100~500GS.
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| CN110828094A (en) * | 2019-11-13 | 2020-02-21 | 黑龙江省科学院高技术研究院 | Preparation method of magnetic fluid for high-magnetic-sedimentation-resistance sealing under strong magnetic field condition |
| CN114628143A (en) * | 2022-04-06 | 2022-06-14 | 黑龙江工程学院 | Preparation method of low-volatility high-temperature-resistant magnetic fluid |
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| CN110828094A (en) * | 2019-11-13 | 2020-02-21 | 黑龙江省科学院高技术研究院 | Preparation method of magnetic fluid for high-magnetic-sedimentation-resistance sealing under strong magnetic field condition |
| CN110828094B (en) * | 2019-11-13 | 2021-05-14 | 黑龙江省科学院高技术研究院 | Preparation method of magnetic fluid for high-magnetic-sedimentation-resistance sealing under strong magnetic field condition |
| CN114628143A (en) * | 2022-04-06 | 2022-06-14 | 黑龙江工程学院 | Preparation method of low-volatility high-temperature-resistant magnetic fluid |
| CN114628143B (en) * | 2022-04-06 | 2022-11-25 | 黑龙江工程学院 | Preparation method of low-volatility high-temperature-resistant magnetic fluid |
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