CN107039139B - A kind of preparation method of magnetic fluid and its magnetic fluid of preparation - Google Patents
A kind of preparation method of magnetic fluid and its magnetic fluid of preparation Download PDFInfo
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- CN107039139B CN107039139B CN201710307740.3A CN201710307740A CN107039139B CN 107039139 B CN107039139 B CN 107039139B CN 201710307740 A CN201710307740 A CN 201710307740A CN 107039139 B CN107039139 B CN 107039139B
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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
- H01F1/442—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 metal or alloy, e.g. Fe
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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
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Abstract
The invention discloses a kind of preparation method of magnetic fluid and its magnetic fluids of preparation, it is therefore intended that solves when addition oleic acid is modified magnetic-particle, oleic acid is excessive, does not carry out the problem of single layer coats subsequent processing to magnetic-particle.The preparation method includes the following steps: magnetic powder preparation, magnetic powder single layer cladding, magnet dispersion.The present invention changes the surface-active of magnetic-particle in magnetic-particle surface success grafted hydrophobic surface active groups, and has carried out the processing of single layer cladding to magnetic-particle, effectively avoids the problem of oleic acid excess, has preferable effect.Meanwhile the present invention provides a kind of magnetic fluid of activating agent containing second surface, by the adjustment to component, effectively prevents the use of poisonous and harmful substance, environmentally protective, wide adaptability can be used for the dispersion of a variety of magnetic fluid base fluids, and application prospect is good.
Description
Technical field
The present invention relates to field of nanometer material technology, especially Surface Modification of Nanosized Materials and field of dispersions, specially a kind of magnetic
The preparation method of fluid and its magnetic fluid of preparation.
Background technique
Magnetic fluid, also known as magnetic liquid, ferrofluid or magnetic liquid are one invented by Nasa the 1960s
Kind new function material is mainly magnetic nanoparticle, base load liquid and the surface of nanometer scale (10nm or less) by diameter
Activating agent three parts composition.Nanoparticle forms one by interfacial agent with base load liquid, even if in gravitational field, electric field, magnetic
Can also exist steadily in the long term under field action, not generate and precipitate and separate；Therefore, it is widely used in chemical industry, biology and clinic
The multiple fields such as medicine.
The surfactant of magnetic-particle adsorption includes two kinds of adsorption mechanisms: first is that chemisorption, this is inhaled to stablize
It is attached；Second is that physical absorption, which cannot be stabilized, and under the more harsh operating condition of environment, lead to magnetic fluid separation not
It can be stabilized, directly affect the stability of industrial part.
George et al. (U.S.3843540) utilizes coprecipitation magnetic nanoparticle, surface-modified to be prepared for magnetic
Fluid, operation is concise, also greatly shortens on the time, more traditional polishing (patent U.S.3215572 and U.S.148206) letter
Easily, energy saving, it is conducive to industrial application.However, they come with some shortcomings during preparing magnetic fluid: 1) oleic acid is being added to magnetic
Property particle when being modified, oleic acid is excessive, but to the subsequent processing of magnetic-particle progress single layer cladding；2) prepared by magnetic fluid
After good, due to dealing with improperly, so that magnetic fluid can not be steady in a long-term.
The country, in " magnetic liquid theoretical and application " book of Li Decai professor, the preparation process of kerosene based magnetofluid is obtained
It to some improvement, but does not mention equally yet and removes magnetic-particle surface physics adsorption layer, i.e., without carrying out the processing of single layer cladding.
The student Lv Jianqiang of Li Decai once in his Master's thesis " nano-magnetic fluid preparation and performance study ", referred to how solving
The problem of surfactant is added in right amount, but do not provide actual characterization and as a result, mentioned in text it is appropriate be also root
Determine according to experiment effect, actual effect explanation cumbersome and without single layer cladding.
And the preparation of the magnetic fluid slightly higher for Matrix viscosity, such as diester based magnetofluid, total loss system oil base
Serial magnetic fluid or more highly viscous pump oil based magnetofluid, then need to add second surface activating agent, second of surface-active
Agent directly affects the dispersibility of particle and other performances of magnetic fluid.Use for second surface activating agent also occurs more
Kind different selection, such as nonylphenol polyoxyethylene ether (US4956113), amine surfactants etc., these surfactants
There is contact injury to human body, and minute quantity can cause water body seriously to pollute.
For this purpose, there is an urgent need to a kind of new methods or product, to solve the above problems.
Summary of the invention
Goal of the invention of the invention is: for when addition oleic acid is modified magnetic-particle, oleic acid is excessive, does not have
The problem of carrying out single layer cladding subsequent processing to magnetic-particle, provides a kind of preparation method of magnetic fluid and its magnetic current of preparation
Body.The present invention changes the surface-active of magnetic-particle in magnetic-particle surface success grafted hydrophobic surface active groups, and
The processing of single layer cladding has been carried out to magnetic-particle, the problem of oleic acid excess has effectively been avoided, there is preferable effect.Meanwhile this hair
A kind of bright magnetic fluid for providing activating agent containing second surface effectively prevents poisonous and harmful substance by the adjustment to component
It uses, environmentally protective, wide adaptability can be used for the dispersion of a variety of magnetic fluid base fluids, and application prospect is good.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of magnetic fluid, includes the following steps:
(1) prepared by magnetic powder
By Fe3+With Fe2+The wiring solution-forming of 1:1.5 ~ 2 in molar ratio, and concentrated ammonia liquor is added thereto, until black precipitate is complete
Until full generation, the first black precipitate solution is obtained；
(2) magnetic powder single layer coats
Gained the first black precipitate solution is rapidly heated to 80 ~ 100 DEG C, and oleic acid and low-carbon alkanes are added thereto,
Stirring is obviously layered to solution, and obtains magnetic current body fluid using the method for dipping magnetic inclination analysis, magnetic current body fluid is centrifuged, deionized water
After cleaning, organic solvent flocculation, then carries out cryogenic vacuum and dry the magnetic powder coated to get single layer；
(3) magnet disperses
The magnetic powder of the cladding of single layer obtained by step (2) is weighed, and the magnetic powder of single layer cladding is added in base fluid at normal temperature, is stirred
It mixes and is dispersed to no precipitating, then be centrifuged, the liquid poured out after centrifugation is magnetic fluid；
Or the magnetic powder of the cladding of single layer obtained by step (2) is taken, and be at normal temperature dispersed with stirring the magnetic powder that single layer coats
In intermediate fluid, the second intermediate solution is obtained, and the second intermediate solution is upgraded to rapidly to 140 ~ 170 DEG C, then is added thereto poly-
Isobutene succimide, base load liquid, are uniformly mixed, until be cooled to room temperature after intermediate fluid is volatilized completely, then carry out from
The heart, the liquid poured out after centrifugation are magnetic fluid.
In the step 1, by Fe3+With Fe2+The wiring solution-forming of 1:1.5 ~ 2 in molar ratio, and solution is warming up to 25 ~ 60 DEG C,
Concentrated ammonia liquor is added thereto again, until black precipitate generates completely, obtains the first black precipitate solution.
In the step 1, the concentration of ammonium hydroxide is 25% ~ 28%；With Fe3+Molar amount, the additional amount of ammonium hydroxide is 400 ~
700ml/mol Fe3+。
In the step 2, low-carbon alkanes are kerosene.
In the step 2, when single flocculates, the volume of organic solvent is 2 ~ 4 times of magnetic current body fluid volume.
In the step 2, flocculated using acetone.
In the step 3, the additional amount of intermediate fluid is 3 ~ 6 times of the magnetic powder weight of weighed single layer cladding.
In the step 3, intermediate fluid is low boiling point hydrocarbon.
In the step 3, intermediate fluid is the hydrocarbon of C4 ~ C10.
In the step 3, intermediate fluid is one of hexane, heptane or a variety of.
In the step 3, base fluid is low-carbon oil product；In terms of the magnetic powder of weighed single layer cladding, the volume that base fluid is added is
The magnetic powder of 0.8mL/g-2mL/g single layer cladding.
The low-carbon oil product is one of kerosene, diesel oil or a variety of.
In the step 3, the additional amount of polyisobutene succinimide is the magnetic powder weight of weighed single layer cladding
20%-50%。
In the step 3, base load liquid be one of two esters base load liquid, hydraulic oil, total loss system oil, pump oil or
It is a variety of.
In the step 3, in terms of the magnetic powder of weighed single layer cladding, the volume that base load liquid is added is 0.4mL/g-2mL/g
The magnetic powder of single layer cladding.
Using magnetic fluid prepared by preceding method.
For foregoing problems, the present invention provides a kind of preparation method of magnetic fluid and its magnetic fluid of preparation.In the present invention,
Magnetic powder is prepared first: magnetic powder is prepared according to chemical coprecipitation, by Fe2+:Fe3+The solution of massage 1:1.5 ~ 2 rises to 25-60 DEG C, adds
Enter concentrated ammonia liquor, until black precipitate generates completely, obtains the first black precipitate solution.Further, the concentration of ammonium hydroxide is 25%-
28%, additional amount 400-700ml/molFe3+。
Secondly, carrying out magnetic powder single layer cladding: the first obtained black precipitate being rapidly heated to 80 DEG C ~ 100 DEG C, is added suitable
Oleic acid and low-carbon small molecule alkane (such as kerosene) are measured, and accelerates to stir, depressurization after 3-8 minutes (by taking kerosene as an example,
Fluid-tight is formed before stirring, after agitated, fluid-tight is destroyed, i.e. depressurization), continue stirring and be obviously layered to mixed solution, so
Use strong magnetic separation afterwards, then outwell supernatant, tentatively obtain magnetic fluid A, magnetic fluid A is centrifuged, deionized water is cleaned repeatedly,
Again after acetone flocculates repeatedly, vacuum drying coats under low temperature to get single layer magnetic powder.Further, with Fe3+Meter, oleic acid dosage
For 40-110ml/molFe3+, acetone volume is 2-4 times of magnetic fluid A volume.
Finally, for the magnetic fluid of low-carbon base fluid, the magnetic powder of the single layer cladding of preparation is weighed, under room temperature, stir in base fluid
It mixes and is dispersed to no precipitating, be then centrifuged, pour out liquid, magnetic fluid can be obtained.Wherein, base load liquid can be low for kerosene, diesel oil etc.
The 0.8mL/g-2mL/g that volume is magnetic dry powder weight is added in carbon oil product.Using which, first surface activating agent is made
The magnetic fluid of (oleic acid) cladding.
And esters biggish for carbon content, hydraulic oil, pump oil etc., the magnetic powder of the single layer cladding of preparation is weighed, under room temperature,
It is dispersed with stirring in intermediate fluid, is brought rapidly up to 140 ~ 170 DEG C, the uniform mixed liquor of T154A and base load liquid is added and quickly stirs
It mixes, after 20-30min, until intermediate fluid is volatilized completely, is cooled to room temperature, high speed centrifugation is to obtain uniform magnetic fluid.Wherein, in
Between liquid can be low-boiling hydrocarbon, such as (just) heptane or (just) hexane etc., the quality of T154A is magnetic powder weight
20%-50%.Wherein, base load liquid can be two esters, hydraulic oil, total loss system oil, pump oil etc., and it is magnetic dry that volume, which is added,
The 0.4mL/g-2mL/g of powder weight.Using which, first surface activating agent (oleic acid), second surface activating agent is made
(T154A) magnetic fluid coated.
In the magnetic fluid of hydrocarbon, the dosage of surfactant of coated magnetic particle is appropriate, if very little
It is then not enough to form complete wrapping layer；It is too many then formed multilayer absorption, instead resulting in stability and magnetism can decline.Guaranteeing
In the case where first clad, that is, chemisorbed layer energy coated magnetic particle completely, in order to eliminate the object that cannot be stabilized as far as possible
Adsorption layer is managed, invention increases being cleaned repeatedly to modified nano particle, before the increased step can make
The dosage for the surface modifier that phase is added is without exact requirements, as long as surfactant is slightly excessive, to meet complete chemistry package
Layer can complete coated magnetic particle.On the one hand the increase step can simplify the dosage control difficulty that surfactant is added；
On the other hand, the surfactant (physical absorption layer) that removing that can be more as far as possible cannot be stabilized, reaches magnetic-particle surface
It is coated to single layer.
And needing to carry out twice-modified magnetic fluid for diester, pump oil base etc., the present invention selects polyisobutene succinyl
Imines (T154A) disperses oil product, which belongs to environmentally friendly machine to human body and the equal fanout free region of environment.Pass through reality
Test is fixed, and in magnetic fluid of the present invention using polyisobutene succinimide preparation, polyisobutene succinimide is to oil product
Favorable dispersibility, magnetic fluid are functional；Compared with existing similar product on the market, saturation magnetization data of the invention
Quite, with good application prospect.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1) present invention provides a kind of short-cut method of nano magnetic particle surface modification suitable for a variety of base fluids, in magnetism
Particle surface success grafted hydrophobic surface active groups, change the surface-active of magnetic-particle；
2) present invention can improve the purity of magnetic fluid, increase the stability and magnetism energy of magnetic fluid, have preferable application
Prospect；
3) it is effectively kept away for the magnetic fluid for needing to add second surface activating agent by the adjustment to component in the present invention
The use of poisonous and harmful substance is exempted from, environmentally protective, wide adaptability can be used for the dispersion of a variety of magnetic fluid base fluids, application prospect
It is good；
4) magnetic fluid prepared by the present invention, saturation magnetization is higher, and good performance is able to satisfy different application demands,
With good application prospect.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
Fig. 1 is the hysteresis loop of the magnetic fluid prepared in embodiment 2.
Fig. 2 is the hysteresis loop of the magnetic fluid prepared in embodiment 1.
Fig. 3 is the hysteresis loop of the hydraulic oil-based magnetic fluids prepared in embodiment 3.
Fig. 4 is the hysteresis loop of the SK-3 diffusion pump oil based magnetofluid prepared in embodiment 4.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
Embodiment 1
It is as follows that the present embodiment prepares the step of magnetic fluid.
1) Fe is pressed3+And Fe2+Molar ratio be Fe3+: Fe2+=1:1.5-2 configures solution, and the solution is placed in 20-
It in 60 DEG C of water-baths, mixes slowly, while instilling the concentrated ammonia liquor that concentration is 25%-28%, control the time for adding of ammonium hydroxide in 5-8min/
L generates precipitating, obtains the first black precipitate solution until fully reacting.
2) the first black precipitate solution is moved into 95 DEG C of water-bath, accelerates stirring, while oleic acid and small point of low-carbon is added
Sub- alkane stirs 3-8min；Then, after being slowly stirred 25min, mixing liquid is poured out, dipping magnetic inclination analysis is outwelled supernatant, obtained down
Layer magnetic current body fluid C.Magnetic current body fluid C is centrifuged 30min under 4500r/min revolving speed, is cleaned with deionized water, which repeats 3
It is secondary；It is flocculated again with acetone, with strong magnetic separation, outwells supernatant, which repeats 3 ~ 5 times；Carry out again cryogenic vacuum drying to get
The magnetic powder D of single layer cladding.
3) the magnetic powder D of single layer cladding is weighed, is added in low-carbon alkanes (using heptane in the present embodiment), is slowly stirred
20min obtains mixture F；The mixture of T154A and DOS(dioctyl sebacate) is added in mixture F, stirring is accelerated
After 30min, the second intermediate solution H is obtained.Second intermediate solution H is moved into oil bath, since temperature is greater than the boiling of low-carbon alkanes
Point persistently stirs 30min, discharges low-carbon alkanes, continues to pour out after stirring 90min to get diester based magnetofluid, hysteresis loop is shown in
Shown in Fig. 2.Fig. 2 is diester based magnetofluid hysteresis loop, it can be seen that saturation magnetization from its bottom data
Magnetization(Ms)=347.24Gs.Through actual verification, diester based magnetofluid manufactured in the present embodiment after 2 years according to
It so keeps stablizing.
Embodiment 2
The magnetic powder D of single layer cladding is prepared according to step 2 in embodiment 1.The magnetic powder D of single layer cladding is weighed, and kerosene is added
In, it quickly stirs until no precipitate, obtains mixture E；By mixture E at 4500rpm/min high speed centrifugation, stablized
Magnetic fluid (i.e. kerosene based magnetofluid), hysteresis loop is as shown in Fig. 1.Fig. 1 is kerosene based magnetofluid hysteresis loop, from it
It can be seen that saturation magnetization Magnetization (Ms)=685.76Gs in bottom data.Through actual verification, the present embodiment system
Standby kerosene based magnetofluid being capable of stable for extended periods of time.
Meanwhile the simple substance kerosene of the present embodiment is replaced with other hydrocarbon compounds, the carbon of corresponding base fluid can be prepared
Hydrogen species magnetic fluid.
Embodiment 3
It changes the DOS base fluid in embodiment 1 into hydraulic oil, hydraulic oil-based magnetic fluids can be obtained, other and 1 phase of embodiment
Together.The hysteresis loop for the hydraulic oil-based magnetic fluids that the present embodiment is prepared is as shown in Fig. 3.Fig. 3 is hydraulic oil-based magnetic fluids magnetic
Hysteresis curves, it can be seen that saturation magnetization Magnetization (Ms)=418.74Gs from its bottom data.Through actual verification,
Hydraulic oil-based magnetic fluids manufactured in the present embodiment being capable of stable for extended periods of time.
Embodiment 4
It changes the DOS base fluid in embodiment 1 into SK-3 diffusion pump oil, SK-3 diffusion pump oil based magnetofluid can be obtained,
He is same as Example 1.
The hysteresis loop for the SK-3 diffusion pump oil based magnetofluid that the present embodiment is prepared is as shown in Fig. 4.Fig. 4 is pump oil base
Magnetic fluid hysteresis loop, it can be seen that saturation magnetization Magnetization (Ms)=84.298Gs from its bottom data.Through
Actual verification, pump oil based magnetofluid manufactured in the present embodiment being capable of stable for extended periods of time.
In the present embodiment, DOS can be replaced into other diester, such as dioctyl adipate (DOA) etc., can prepare corresponding base
Two esters magnetic fluids of liquid；It changes total loss system oil into, then can prepare the total loss system oil series magnetic current of corresponding base fluid
Body.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
1. a kind of preparation method of magnetic fluid, which comprises the steps of:
(1) prepared by magnetic powder
By Fe3+With Fe2+The wiring solution-forming of 1:1.5~2 in molar ratio, and concentrated ammonia liquor is added thereto, until black precipitate is completely raw
As only, the first black precipitate solution is obtained；
(2) magnetic powder single layer coats
Gained the first black precipitate solution is rapidly heated to 80~100 DEG C, and oleic acid and low-carbon alkanes are added thereto, stirring
It is obviously layered to solution, and the method for using dipping magnetic inclination analysis obtains magnetic current body fluid, and magnetic current body fluid is centrifuged, deionized water is clear
It washes, after organic solvent flocculation, then carries out cryogenic vacuum and dry the magnetic powder coated to get single layer；
(3) magnet disperses
The magnetic powder of the cladding of single layer obtained by step (2) is weighed, and the magnetic powder of single layer cladding is added in base fluid at normal temperature, stirring point
It is dissipated to no precipitating, then is centrifuged, the liquid poured out after centrifugation is magnetic fluid；
Or the magnetic powder of the cladding of single layer obtained by step (2) is taken, and the magnetic powder that single layer coats is dispersed with stirring in centre at normal temperature
In liquid, the second intermediate solution is obtained, and the second intermediate solution is upgraded to rapidly to 140~170 DEG C, then poly- isobutyl is added thereto
Alkene succimide, base load liquid, are uniformly mixed, until being cooled to room temperature after intermediate fluid is volatilized completely, then are centrifuged, from
The liquid poured out after the heart is magnetic fluid.
2. the preparation method of magnetic fluid according to claim 1, which is characterized in that in the step 1, by Fe3+With Fe2+Massage
You are warming up to 25~60 DEG C than the wiring solution-forming of 1:1.5~2, and by solution, then concentrated ammonia liquor is added thereto, until black precipitate is complete
Until full generation, the first black precipitate solution is obtained.
3. the preparation method of magnetic fluid according to claim 2, which is characterized in that in the step 1, the concentration of ammonium hydroxide is
25%~28%；With Fe3+Molar amount, the additional amount of ammonium hydroxide is 400~700ml/mol Fe3+。
4. the preparation method of magnetic fluid according to claim 1, which is characterized in that in the step 2, low-carbon alkanes are coal
Oil.
5. the preparation method of magnetic fluid according to claim 1, which is characterized in that in the step 3, the additional amount of intermediate fluid
It is 3~6 times of the magnetic powder weight of weighed single layer cladding.
6. the preparation method of magnetic fluid according to claim 5, which is characterized in that in the step 3, intermediate fluid is low boiling point
Hydrocarbon.
7. the preparation method of any one of -6 magnetic fluids according to claim 1, which is characterized in that in the step 3, base fluid is
Low-carbon oil product；In terms of the magnetic powder of weighed single layer cladding, the volume that base fluid is added is the magnetic of 0.8mL/g-2mL/g single layer cladding
Powder.
8. the preparation method of any one of -6 magnetic fluids according to claim 1, which is characterized in that in the step 3, poly- isobutyl
The additional amount of alkene succimide is the 20%-50% of the magnetic powder weight of weighed single layer cladding.
9. the preparation method of any one of -6 magnetic fluids according to claim 1, which is characterized in that in the step 3, base load liquid
For one of two esters base load liquid, hydraulic oil, total loss system oil, pump oil or a variety of.
10. magnetic fluid prepared by any one of -9 the methods according to claim 1.
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| CN107610874A (en) * | 2017-10-18 | 2018-01-19 | 方利俊 | A kind of water-base magnetic liquid and preparation method thereof |
| CN107492434A (en) * | 2017-10-18 | 2017-12-19 | 方利俊 | It is a kind of using flaky calcium carbonate as water-base magnetic liquid of template and preparation method thereof |
| CN110400690B (en) * | 2019-08-01 | 2020-09-04 | 浙江鑫盛永磁科技有限公司 | Magnetic fluid preparation method convenient for filtering |
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| CN104465008A (en) * | 2014-11-18 | 2015-03-25 | 成都理想财富投资咨询有限公司 | Magnetic fluid preparation method for DNA purification |
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| CN1414075A (en) * | 2002-09-25 | 2003-04-30 | 重庆仪表材料研究所 | Stable magnetic rheological liquid and its preparation method |
| JP2007165482A (en) * | 2005-12-12 | 2007-06-28 | Inst Nuclear Energy Research Rocaec | Method of preparation of oily magnetic fluid |
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