CN106486240B - The Preparation equipment and method of nanometer magneto-rheological fluid - Google Patents
The Preparation equipment and method of nanometer magneto-rheological fluid Download PDFInfo
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Abstract
The present invention relates to the preparation method of nanometer magneto-rheological fluid and devices.The device of preparation nanometer magneto-rheological fluid includes: ball mill, and ball mill is for providing the primary magnetic particle comprising nano magnetic particle by ball milling magnetic powder materials；Positioned at ball mill downstream and the separator that is connected with ball mill, separator therefrom isolates the main secondary magnetic particle comprising nano magnetic particle in required particle size range for receiving the primary magnetic granular materials from ball mill；With the blender for being located at separator downstream and being connected with separator, blender is for mixing secondary magnetic particle with carrier fluid and additive, to obtain a nanometer magneto-rheological fluid.Nanometer magneto-rheological fluid provided by the invention has a huge irreplaceable advantage, for example, without magnetic hysteresis, be not easy to precipitate, viscosity is low, the clear-cut advantages such as quick of, long service life low to component wear rate, high reliablity, response.Invention further discloses the methods of preparation nanometer magneto-rheological fluid.
Description
Technical field
The present invention relates to nanometer magneto-rheological fluid fields.Specifically, the present invention relates to nanometer magneto-rheological fluids.The present invention
Further relate to the equipment and technique of preparation nanometer magneto-rheological fluid.
Background technique
Magneto-rheological fluid is one kind as the changed liquid of its viscosity occurs in magnetic field.By high magnetic permeability, low hysteresis
Soft magnetic granules by the even action of surfactant be scattered in non-magnetic carrier fluid constitute stable suspersion liquid system.
The working principle of magneto-rheological fluid is: under the action of externally-applied magnetic field, each particle is all polarized to magnetic dipole, each dipole
Son attracts each other, and the chain fascicular texture formed between two pole plates crossbearer as bridge is hindering fluid just between pole plate
Often flowing makes it generate the feature of class solid.When removing externally-applied magnetic field, fluid is restored to original state again, i.e., magnetorheological
Liquid carries out the conversion of Rapid reversible between liquid and solid-state.Solid state degree and current strength are at reversible relationship is stablized, i.e.,
Control current strength can accurately control the shear yield strength of solid state magnetorheological fluid.
Researcher is a lot of for many years for magneto-rheological fluid, is also gradually applied to control damping force in various devices at present,
Such as damper, shock absorber, human body artificial limb and resilient seat.Rheology of the magnetorheological fluid under magnetic fields be moment,
Shear yield strength and magnetic field strength after reversible and its rheology have stable corresponding relationship, are very easy to realize intelligence
It can control.Therefore, magnetorheological fluid is a kind of widely used, function admirable intellectual material, and the application field of magneto-rheological fluid is just
It is expanding rapidly.
For traditional magneto-rheological fluid there are hysteresis, being scattered in magneto-rheological fluid has the magnetic-responsive particulate of magnetic hysteresis in magnetic
Magneto-rheological fluid is seted to disturb magneto-rheological fluid from being completely recovered to free-flowing because particle has remanent magnetism after the removal of field
The control process of device work.In order to reduce coercive force, the partial size of the magnetic particle of traditional magneto-rheological fluid is greater than 0.1 μm,
Preferable particle size is greater than 1 μm, and (see United States Patent (USP) US6203717B1 etc.), this just brings another outstanding problem, that is, magnetic particle
It is easily settled in magneto-rheological fluid.
Particle tend to precipitating the reason of first is that oil density (0.7-0.95g/cm3) and metallic particles density (iron
Grain is about 7.86g/cm3) difference is very big, reason second is that larger (its of magnetizable particles partial size in traditional magneto-rheological fluid
Preferential partial size is greater than 1 μm, i.e., 1000 nanometers, such as United States Patent (USP) US6203717B1), micro-solid particle is in fluid media (medium)
Termin al velocity degree and its partial size it is square directly proportional.The sedimentation of material causes the non-uniform Distribution of particle, disturbs
The activity of magneto-rheological fluid.Some early stages magneto-rheological fluid (referring to United States Patent (USP) 2575360,2661825,2886151,
US6203717B1 etc.) the main component speed that is that iron powder and light viscosity oil, these magneto-rheological fluids are easy to precipitate, and precipitates
Rate is accelerated with the rising of temperature.So it is generally necessary to adding various thickeners and suspending agent.Due to these anti-settling components
A large amount of additions, the viscosity of magneto-rheological fluid greatly improved, still, this both increases material no magnetic field state flowing
Resistance (viscosity).
The service life that the sedimentation of magnetic particle directly results in magneto-rheological fluid is short, reliability is low and eventually leads to magnetic current unsteady flow
Body failure.
The initial viscosity of magneto-rheological fluid is big, flow resistance is big, this directly results in example of the equipment component when not adding magnetic field
Such as motion parts or the degraded performance of device.
The presence of magnetic hysteresis is the common fault of the prior art, and this defect can be with using the delay of time more prominent, this is not
It will result only in the poor performance of magneto-rheological fluid and its application apparatus, and especially will cause the control response of fluid or equipment
Performance And Reliability is low, and equally can also have the defects that service life is short.
In addition to particle sedimentation, initial viscosity it is big and there are magnetic hysteresis, existing magneto-rheological fluid there is also another protrusion
The technical issues of be wear problem.The moving component surface that magnetic particle in magneto-rheological fluid can be in contact with it causes to wear, can
The partial size of magnetized particles is bigger, and abrasive wear is more serious.
Therefore, this field needs improved magneto-rheological fluid and its preparation process and equipment with the development of technology, with gram
Take defect in the prior art.
Summary of the invention
The present invention proposes preparation in a creative way and provides nanometer magneto-rheological fluid to solve above-mentioned technical problem and other
Defect in the prior art.The invention also provides the device and method of preparation nanometer magneto-rheological fluid.
If magnetic-responsive particulate there are hysteresis, after the removal of magnetic field because particle has remanent magnetism prevent magneto-rheological fluid from
It is completely recovered to free-flowing, is unfavorable for the control of magneto-rheological fluid device work, this requires the magnetic of magneto-rheological fluid
Responsive particles have alap coercive force.Coercive force is the important parameter for describing the hysteresis of ferromagnetic material.
Coercive force mechanism and the block of material of fine grained magnetic material are not quite similar, the coercive force of ferromagnetic particle seriously according to
Rely the size (see figure 1) in its size.
Fig. 1 shows the coercive force of magnetic particle and the relationship of partial size.In micron range, reduction partial size typically results in strong
The maximum value of the increase of retentiveness, coercive force can be in " single domain " partial size (DSD) in obtain.But when the partial size of magnetic particle subtracts
It is small to below " single domain " partial size when, coercive force is reduced as partial size reduces instead, is faced when the partial size of magnetic particle drops to one
Boundary nanoscale (DSP) below when, coercive force is reduced to zero, and at this moment original ferrimagnet is converted into super paramagnetic material,
Super paramagnetic material i.e. its coercive force is down to substantially zeroed magnetic material.
Fig. 2 shows the single domain partial size (D of part ferromagnetic materialSD) and superparamagnetism conversion partial size (DSP).
If the partial size of magnetic particle is decreased in the range of nanoscale some scale, coercive force astoundingly drops
To substantially zeroed or completely zero, at this moment original ferrimagnet is converted into super paramagnetic material, when these magnetic particles by with
When magneto-rheological fluid, it will be able to obtain the novel nano magneto-rheological fluid of the invention that performance surmounts the prior art completely.
With traditional magneto-rheological fluid (such as United States Patent (USP) 2575360,2661825,2886151,5645752,
Described in the patents such as 7393463B2,6203717B1 and 2006/0033069 A1) it compares, the device of the invention preparation is received
Rice magnetorheological fluid materials have the advantage that
A. without magnetic hysteresis
There are hysteresis for traditional magnetic-responsive particulate, make magneto-rheological fluid not because particle has remanent magnetism after the removal of magnetic field
It can be completely recovered to free-flowing；Meanwhile the magnetization curve of rising is not overlapped with the magnetization curve of decline, influences controller
Control process.Nanometer magnetic-responsive particulate material of the invention has superparamagnetism, that is, coercive force is substantially zeroed, therefore makes
The nanometer magnetic-responsive particulate material obtained is substantially without magnetic hysteresis.
B. not easily settled
Termin al velocity degree of the micro-solid particle in fluid media (medium) and its partial size it is square directly proportional.Traditional magnetic
Responsive particles are in order to reduce remanent magnetism, and preferable particle size is in 1 μm or more (explanation for being detailed in these patents), the grain of material of the present invention
1/50 of diameter less than traditional material, settling velocity in a fluid solve magneto-rheological fluid less than traditional material 1/2500
Particle settlement issues.
C. mitigate the wear rate to component
The partial size of abrasive wear and abrasive grain is closely related, and 1/50 of partial size less than traditional material of material of the present invention can be shown
Write the abrasion reduced to moving component.
D. initial viscosity is low
Because of the low characteristic of nano material sinking speed, it is not necessary that highly viscous anti-settling component is largely added in carrier fluid；Because
Remanent magnetism is not present without hysteresis in nanometer magnetic-responsive particulate of the invention after the removal of magnetic field, magneto-rheological fluid can be restored to certainly
By flow regime.These factors can make the initial viscosity sharp fall of magneto-rheological fluid.
E. the device of the invention can realize continuous production, high production efficiency, and production cost is low.
More specifically, according to the present invention, a kind of nanometer of magneto-rheological fluid is provided, comprising: nanoscale is magnetizable
Magnetic particle, wherein the average grain diameter of the magnetic particle is less than 100 nanometers；With the fluid for being used as carrier fluid, wherein the magnetic particle
Dispersed precipitate is in the fluid；With the additive being added in the fluid.
An embodiment according to the present invention, the partial size of the magnetic particle is in critical nanoscale (DSP) hereinafter, described critical
Nanoscale (DSP) depend on the magnetic particle material type.
An embodiment according to the present invention, nanometer magneto-rheological fluid described in claim 1, which is characterized in that the magnetic
The average grain diameter of particle can be realized superparamagnetism, be, for example, less than 80 nanometers, and preferably smaller than 50 nanometers, such as at 0.1-80 nanometers
More between, preferably between 0.2-50 nanometers, most preferably between 0.5-20 nanometers.
An embodiment according to the present invention, the material of magnetic particle can be selected from iron, ferroalloy, ferrocobalt, ferroplatinum, iron
Oxide, nitrided iron, cementite, carbonyl iron, nickel, cobalt, chromium dioxide, FePt, SmCo, NdFeB, stainless steel, silicon steel, or
The combination of these materials.
An embodiment according to the present invention, the fluid are organic liquids, preferably alpha-olefin.
An embodiment according to the present invention, the fluid also include additive, and the additive is selected from surfactant, divides
Powder, sagging inhibitor, organic thixotropic agents, thickener, antioxidant, lubricant, viscosity modifier, fire retardant, organic clay class
The amount of the combination of rheological additives, sulfur-containing compound and these additives, the additive accounts for magnetorheological fluid composition
Total volume about 0.01% to about 20%, preferably from about 0.01% to about 10%.
The volume of an embodiment according to the present invention, the magnetic particle accounts for total fluid volume about 10% to 70%.
An embodiment according to the present invention, it is viscous in the state of no magnetic field and about 40 DEG C for the nanometer magneto-rheological fluid
Spend about 0.2 to about 1000 centipoise.
An embodiment according to the present invention, the magnetic particle are shape anisotropy and/or magnetocrystalline anisotropy.
The magnetic particle of an embodiment according to the present invention, the shape anisotropy has aspherical shape.
An embodiment according to the present invention, the aspherical shape are selected from sheet, strip, rodlike, cylindric, prism-shaped
Or their any combination.
An embodiment according to the present invention, the sheet or strip are elongated sheet or strip.
An embodiment according to the present invention, the magnetic particle of the magnetocrystalline anisotropy have hexagonal crystal system, cubic system or
The magnetocrystalline structure of rhombohedral crystal.
An embodiment according to the present invention, the magnetizable magnetic particle of nanoscale is the magnetic with superparamagnetism
Grain.
An embodiment according to the present invention, the magnetizable magnetic particle of nanoscale is the core shell knot with encasement
The nano magnetic particle of structure.
An embodiment according to the present invention, the average grain diameter of magnetic particle is in 0.05 DSP-5 DSPBetween, preferably 0.05
DSP-2 DSPBetween, more preferably in 0.05 DSP-1 DSPBetween, most preferably in 0.1 DSP-0.9 DSPBetween select.
According to the present invention, a kind of device for being used to prepare nanometer magneto-rheological fluid is additionally provided, described device includes: ball milling
Machine, the ball mill is for providing the primary magnetic particle comprising nano magnetic particle by ball milling magnetic powder materials；Positioned at ball mill
Downstream and the separator being connected with ball mill, the separator are used to receive the primary magnetic granular materials from ball mill, and
And therefrom isolate the main secondary magnetic particle comprising nano magnetic particle in required particle size range；Be located at separator downstream simultaneously
And the blender being connected with separator, the blender come for mixing secondary magnetic particle with carrier fluid and additive
To nanometer magneto-rheological fluid.
An embodiment according to the present invention, described device are used to prepare the nanometer magneto-rheological fluid with superparamagnetism.
An embodiment according to the present invention, the ball mill are agitating ball mills.
An embodiment according to the present invention, the separator include precipitation and separation device, and the precipitation and separation device is located at ball milling
Machine downstream, for primary magnetic particle to be separated into comprising non-required more coarse grained lower layer's fluid by gravity or centrifugal force and
Top fluid comprising thinner magnetic particle.
An embodiment according to the present invention, the separator further include magnetic separator, and the magnetic separator is located at described heavy
Shallow lake separator downstream is simultaneously attached thereto, for receiving the top fluid comprising thinner magnetic particle from the precipitation and separation device,
And the top fluid is further separated into the fluid containing required secondary magnetic particle by way of adding magnetic field and is contained
The fluid to be recycled of non-required magnetic particle, wherein the fluid containing required secondary magnetic particle is transferred to the stirring
Machine.
An embodiment according to the present invention, the precipitation and separation device are equipped with switchable outlet in its bottom, are used for institute
It states lower layer's fluid and is pumped back to the ball mill.
An embodiment according to the present invention, the magnetic separator are equipped with outlet, are used for the fluid pumped back to be recycled
To the ball mill.
According to the present invention, a kind of method for being used to prepare nanometer magneto-rheological fluid is additionally provided, which comprises by magnetic
Powder raw material, additive and a part of carrier fluid are added to ball mill together and carry out ball milling, to prepare comprising nano magnetic particle
Primary magnetic particle；Primary magnetic particle is delivered to the separator in downstream together with a part of carrier fluid, is contained to isolate
There is the fluid of required secondary magnetic particle, and is sent to the blender in downstream；Carrier fluid stream is further added in blender
Body and antiprecipitant are stirred, to obtain a nanometer magneto-rheological fluid.
The step of embodiment according to the present invention, the separation, includes, by primary magnetic particle together with a part of carrier fluid stream
Body carries out precipitation and separation in precipitation and separation device and obtains the top fluid comprising thinner magnetic particle, then that the top fluid is defeated
It send to magnetic separator.
An embodiment according to the present invention, in the magnetic separator by way of adding magnetic field from the top fluid into
One step isolates the fluid containing required secondary magnetic particle, and the fluid containing required secondary magnetic particle is passed
Transport to the blender.
An embodiment according to the present invention, the method is by means of dress described in any one of 4-20 according to claim 1
It sets to prepare a nanometer magneto-rheological fluid.
An embodiment according to the present invention, the additive include surfactant and defoaming agent.
Compared with traditional magneto-rheological fluid, nanometer magneto-rheological fluid of the invention has huge irreplaceable excellent
Gesture, for example, without magnetic hysteresis, be not easy to precipitate, viscosity is low, long service life low to component wear rate, high reliablity, response are clear-cut fast
The performance advantages such as speed.
Magneto-rheological fluid of the invention can be applied to (but being not limited to) damper, buffer, damper, shock absorber,
The devices such as human body artificial limb and resilient seat and device.
Detailed description of the invention
By reading this specification in conjunction with the following drawings, features, objects and advantages of the invention will become more to show and easy
See, in the accompanying drawings:
Fig. 1 shows the coercive force of magnetic particle and the relationship of partial size.
Fig. 2 illustrates the single domain partial size (D of part ferromagnetic materialSD) and superparamagnetism conversion partial size (DSP).
Fig. 3 is the schematic isometric of the device according to an embodiment of the invention for being used to prepare nanometer magneto-rheological fluid
Figure.
Fig. 4 is the schematic plan view that the embodiment of device of nanometer magneto-rheological fluid is used to prepare described in Fig. 3.
Specific embodiment
In the description below to the drawings and specific embodiments, the thin of one or more embodiments of the invention will be illustrated
Section.From these description, attached drawing and claims, other features, objects, and advantages of the present invention can be understood.
Several specific embodiments of the invention will be described in more detail below.
Before further describing embodiments of the present invention, the present inventor wants to illustrate several terms of the invention as follows.
In the present invention, term " anisotropy " has the meaning of several aspects.
First, term " anisotropy " can represent each to different of the vpg connection of the nano magnetic particle in magneto-rheological fluid
Property, this anisotropy can enable the nano magnetic particle after applying magnetic field quickly to tie with stronger binding force and twisting resistance
Chain is synthesized, it is simply quick to the response of externally-applied magnetic field, and the reset condition after removing externally-applied magnetic field before fast quick-recovery.Phase
Than under, for example, existing magnetic particle, such as the magnetic particle of Lord company of the U.S., not only size is big, such as up to 1 micron of left side
The right side, and its magnetic particle generally show it is spherical or substantially spherical so that the response to externally-applied magnetic field is slow.
Since the size of the magnetic particle in magneto-rheological fluid is in the range of nanoscale, the presentation of nano magnetic particle is each
The shape of anisotropy belongs to micro-shape, needs in the state of enough amplifications, such as can be clearly at SEM or TEM
Show.Such as, but not limited to, the shape of the presentation " anisotropy " of nano magnetic particle is preferably aspherical shape, including but not
It is limited to sheet, strip, rodlike, column, prism-shaped, cylinder etc..The present inventor is astoundingly sent out by test
Existing, preferably the nano magnetic particle of sheet or strip is convenient for the quick chaining after externally-applied magnetic field and makes magneto-rheological fluid with excellent
Torsional property more, in particular, the nano magnetic particle of elongated sheet or strip is preferred.
Second, term " anisotropy " can represent each to different of the magnetocrystalline structure of the nano magnetic particle in magneto-rheological fluid
Property.The present inventor surprisingly it has been found that nano magnetic particle different magnetocrystalline structures, can be to nano magnetic particle outside
The performance of such as responsiveness and quick chaining performance and antitorque aspect after adding magnetic field makes a significant impact.With it is isotropic
Magnetocrystalline structure is compared, and the nano magnetic particle with anisotropic magnetocrystalline structure can be in such as responsiveness and quick chaining
Energy, torsional strength etc. provide more superior performance.For example, in this respect, face-centered cubic (fcc), body-centered cubic structure
(bcc) crystal structure is considered to be isotropic magnetocrystalline structure, therefore is not preferred.As a comparison, isotropic
Magnetocrystalline structure, such as hexagonal crystal system, part cubic system, rhombohedral crystal equimagnetic crystal structure are capable of providing significant improvement after externally-applied magnetic field
Performance, be therefore preferred.
In the present invention, those skilled in the art are appreciated that term " superparamagnetic ", " superparamagnetism " refer to completely
, it is not in hysteresis that the remanent magnetism and coercive force of magnetic particle are substantially zeroed.
Traditional magneto-rheological fluid technology of preparing cannot make the partial size of magnetic particle be less than superparamagnetism conversion partial size (DSP), it is
Reduction remanent magnetism, the preferable particle size of magnetic particle 1 μm or more (referring to patents such as US 6203717B1), thus bring it is easily settled,
Viscosity is high and the problems such as to component wear.
The device of the invention combines precipitation and separation with high-energy ball milling, using the relationship of particle sinking speed and partial size,
It is automatically separated out satisfactory particle, and auto-returned ball mill is continued to grind by undesirable coarse granule, to make
The partial size of standby magneto-rheological fluid-nanometer magneto-rheological fluid novel out, this fluid magnetic-responsive particulate can be converted lower than superparamagnetism
Partial size DSP(being obtained by adjusting deposition condition), therefore can show super-paramagnetic properties, with no magnetic hysteresis, anti-settling, just
Beginning viscosity is low and to the low characteristic of component wear rate.
The selection of superparamagnetic nanometer magnetic-responsive particulate material
Known any solid with high magnetic saturation intensity may be used to the present invention, specifically include paramagnetism, super suitable
Magnetic and ferromagnetic element and compound.For example, the example of suitable magnetizable particles includes iron, ferroalloy (alloying element packet
Include aluminium, silicon, cobalt, nickel, vanadium, molybdenum, chromium, tungsten, manganese and/or copper), ferriferous oxide (including Fe2O3 and Fe3O4), nitrided iron, carbonization
Iron, carbonyl iron, nickel, cobalt, chromium dioxide, stainless steel and silicon steel.For example, the example of suitable particles include straight iron powder, reduced iron powder,
The mixture of brown iron oxide and straight iron powder.The magnetic-responsive particulate preferentially selected is pure iron and ferrocobalt.
The selection of superparamagnetic nanometer magnetic-responsive particulate partial size
The average grain diameter of magnetic-responsive particulate of the present invention is nanoscale, and preferable particle size is less than the superparamagnetic of selected materials
Property conversion partial size (DSP), preferably average particle size range can be between 0.1DSP-DSP.
The preparation method of superparamagnetic nanometer magnetic-responsive particulate
The preparation method of superparamagnetic nanometer magnetic-responsive particulate material may include but be not limited to coprecipitation method, polyhydric alcohol solutions chemistry
Synthetic method, chemical reduction method, aqueous solution reduction method, polyol reduction method, sol-gel method, hydro-thermal method, ball-milling method etc..
Carrier fluid
The continuous phase of carrier fluid composition magneto-rheological fluid.Nonvolatile, nonpolar organic oil can be employed as carrier liquid component, close
Suitable carrier fluid example includes silicone oil, hydraulic oil, machine oil, gear case oil, alpha-olefin etc..Carrier fluid also includes additive, it may include:
Organic clay, organic thixotropic agents
1. addition organic clay, organic thixotropic agents can control the viscosity of magneto-rheological fluid, flow, delay magnetisable
The sedimentation of particle.Selectable organic clay example includes tallow bentonite, 2- methyl -2- hydrogenated tallow bentonite ammonium salt, 2-
The muddy stone ammonium salt of methyl -2- hydrogenated tallow water.Optional organic thixotropic agents can be 100 rheologic additive of Advitrol and
Thixatrol ST, 1 Rheox rheologic additive etc..
2. antisettling agent
Addition antisettling agent to prevent the sedimentations of nanometer magnetizable particles, optional sagging inhibitor include M-P-A 2000X,
M-P-A 60X antisettling agent or Y-25, Y-40, YPA-100 antisettling agent etc..
3. metallic soap
Other thickeners include that metallic soap includes aluminum stearate, (different) aluminium octoate and pulpous state calcium linoleate, together with solvent
Gel structure is generated, the suspension of magneto-rheological fluid is improved.
4. other additives
According to the purposes of magneto-rheological fluid, other addition additives can be also added, including dispersing agent, surfactant, anti-
Oxidant, lubricant etc..
The preparation for the nanometer magneto-rheological fluid that the invention will now be further described with reference to specific embodiments.
Below with reference to the accompanying drawings the present invention is further described and in conjunction with specific embodiments.
Referring to Fig. 3 and Fig. 4, wherein Fig. 3 is according to an embodiment of the invention to be used to prepare a nanometer magneto-rheological fluid
Device schematic perspective view, Fig. 4 be used to prepare described in Fig. 3 the device of nanometer magneto-rheological fluid embodiment it is schematic
Plan view, an embodiment of the preparation facilities of nanometer magneto-rheological fluid according to the present invention include agitating ball mill 1, precipitation and separation
Device 2, magnetic separator 3, pump 5, blender 4, wherein precipitation and separation device 2 is preferably placed at the downstream of agitating ball mill 1 and passes through pipe
Line 6 is connected with agitating ball mill 1, and magnetic separator 3 is preferably placed at the downstream of precipitation and separation device 2 and also by pipeline and precipitating point
It is connected from device 2.Wherein, magnetic separator 3 and precipitation and separation device 2 are preferably each provided with outlet and agitating ball mill 1, to pass through pump
7 are selectively handled undesirable set of raffinate back to agitating ball mill 1 again.
Blender 4 is preferably placed at 3 downstream of magnetic separator and is connected also by pipeline with magnetic separator 3, comes for receiving
From the fluid comprising required nano magnetic particle of magnetic separator 3.
(1) grinding process
Using such as polyhydric alcohol solutions chemical synthesis, by molysite and cobalt salt, soluble in water together to obtain iron cobalt salt-mixture molten
Liquid uses including but not limited to oxalic acid, oxalates or carbonate to utilize precipitating reagent ion and Fe ion and Co ion as precipitating reagent
Reaction generates the sediment of iron cobalt complex salt, obtains ferrocobalt powder through techniques such as solid-liquor separation, drying, calcining, reduction.
By ferrocobalt powder for example obtained by the above method, abrasive media, surfactant such as Tween 80, defoaming agent
Such as n-butanol, according to a certain percentage (weight ratio are as follows: 70:29:0.9:0.1 supplements n-butanol to the reasonable quantity of visual foam)
It is incorporated an example model JQM-500 of agitating ball mill 1(agitating ball mill 1) in, it is ground with the ratio of grinding media to material of 10:1.This
The revolving speed of kind agitating ball mill 1 is high, and abrasive power is big, therefore grinding efficiency is also higher.
It preferably, can be by circulating pump, to realize that slurry circulation is ground, to improve magnetic powder material utilization rate.
According to an embodiment, alpha-olefin can be used as abrasive media, surfactant can also make dispersing agent simultaneously, prevent
Magnaglo conglomeration and welding.The use of defoaming agent is intended to eliminate the bubble generated because surfactant is added.
(2) precipitation and separation process
It will pass through in the slurry pipeline transport to precipitation and separation device 2 of ball milling, for example, homemade gravity separator or centrifuge separation
Device (model LW50*1100), it (is, for example, less than 50 nanometers of particle size range, grain that partial size, which is met the requirements, using gravity or centrifugal force
The size or range of diameter can be required according to specific magnetic powder type, technique and the requirement of application and it is different) nano magnetic
Grain is separated, which is sent to magnetic separator 3；And partial size it is undesirable (such as partial size be greater than 50
Nanometer) thick magnetic particle send agitating ball mill 1 back to pump circulation and continue to grind.
According to a preferred embodiment, the slurry by ball milling in gravity separator or whizzer can be heated to centainly
Temperature, such as it is heated to 25-50 degrees Celsius, to promote gravity precipitation and separation or centrifuge separation.
(3) Magneto separate process
According to a preferred embodiment, as the additional of gravity precipitation and separation or centrifuge separation, homemade device can be used, benefit
The mode of electromagnetic attraction is generated with exciting current is applied to nano magnetic particle, will be provided with the nano magnetic particle of superparamagnetism from ball
It is further concentrated and separated in grinding media, the nano magnetic particle (medium containing partial mill) isolated can preferably be admitted to blender 4
Carry out lower road agitating procedure.Wherein, the ball-milling medium for isolating nano magnetic particle can be passed through to pump 5 and sent back to via pipeline 7 and stirred
Mix ball mill 1.It according to a preferred embodiment of the invention, can be by the size of control exciting current, to control the magnetic isolated
Powder concentration.
(4) agitating procedure
The slurry for the particle containing nano magnetic isolated from magnetic separator 3 is characterized to the content of magnetic particle, supplement with density value
Antiprecipitant (such as M-P-A2000X, NL chemical company) and lubricant (such as silicone oil), agitated machine 4 is added in alpha-olefin
(model DX-L500) is stirred about 1 hour, and obtains satisfactory nanometer magneto-rheological fluid.
The specific embodiment in conjunction with attached drawing for nanoscale magneto-rheological fluid of the invention, method and apparatus carries out above
Detailed description.It will be understood by those skilled in the art, however, that the above is merely illustrative and describes some specific realities
Mode is applied, to the scope of the present invention, especially the scope of the claims, and does not have any restrictions.
Claims (12)
1. a kind of device for being used to prepare nanometer magneto-rheological fluid, described device include:
Ball mill, the ball mill is for providing the primary magnetic particle comprising nano magnetic particle by ball milling magnetic powder materials；
Positioned at ball mill downstream and the separator that is connected with ball mill, the separator is for receiving the primary from ball mill
Magnetic granular materials, and therefrom isolate the main secondary magnetic particle comprising nano magnetic particle in required particle size range；With
Positioned at separator downstream and the blender that is connected with separator, the blender is used for secondary magnetic particle and carrier fluid stream
Body and additive mixing, to obtain a nanometer magneto-rheological fluid；
Nano magnetic particle in the nanometer magneto-rheological fluid is anisotropic.
2. the apparatus according to claim 1, which is characterized in that described device is used to prepare the nanometer with superparamagnetism
Magneto-rheological fluid.
3. the apparatus according to claim 1, which is characterized in that the ball mill is agitating ball mill.
4. the apparatus according to claim 1, which is characterized in that the separator includes precipitation and separation device, the precipitating point
It is located at ball mill downstream from device, for primary magnetic particle to be separated into comprising non-required relatively coarse granule by gravity or centrifugal force
Lower layer's fluid and top fluid comprising thinner magnetic particle.
5. device according to claim 4, which is characterized in that the separator further includes magnetic separator, the Magneto separate
Device is located at precipitation and separation device downstream and is attached thereto, for receiving from the precipitation and separation device to include thinner magnetic particle
Top fluid, and the top fluid is further separated into containing required secondary magnetic particle by way of adding magnetic field
Fluid and fluid to be recycled containing non-required magnetic particle, wherein the fluid containing required secondary magnetic particle is transmitted
To the blender.
6. device according to claim 4, which is characterized in that the precipitation and separation device is equipped with switchable in its bottom
Outlet, for lower layer's fluid to be pumped back to the ball mill.
7. device according to claim 5, which is characterized in that the magnetic separator is equipped with outlet, and being used for will be described wait return
It receives fluid and is pumped back to the ball mill.
8. a kind of method for being used to prepare nanometer magneto-rheological fluid, which comprises
Magnetic powder materials, additive and a part of carrier fluid are added to ball mill together and carry out ball milling, to prepare comprising nanometer
The primary magnetic particle of magnetic particle；
Primary magnetic particle is delivered to the separator in downstream together with a part of carrier fluid, to isolate containing required
The fluid of secondary magnetic particle, and it is sent to the blender in downstream；
Carrier fluid is further added in blender and antiprecipitant is stirred, to obtain a nanometer magneto-rheological fluid.
9. according to the method described in claim 8, it is characterized in that, the step of separation include, by primary magnetic particle together with
A part of carrier fluid carries out precipitation and separation in precipitation and separation device and obtains the top fluid comprising thinner magnetic particle, then will
The top fluid is delivered to magnetic separator.
10. according to the method described in claim 9, it is characterized in that, in the magnetic separator by way of adding magnetic field from
The top fluid is further separated out the fluid containing required secondary magnetic particle, and contains required secondary magnetic for described
The fluid of particle is transferred to the blender.
11. the method according to any one of claim 8-10, which is characterized in that the method according to right by means of wanting
Device described in any one of 1-7 is sought to prepare a nanometer magneto-rheological fluid.
12. the method according to any one of claim 8-10, which is characterized in that the additive includes surfactant
And defoaming agent.
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| CN201510537836.XA CN106486240B (en) | 2015-08-28 | 2015-08-28 | The Preparation equipment and method of nanometer magneto-rheological fluid |
| EP16840766.6A EP3343573B1 (en) | 2015-08-28 | 2016-08-25 | Nano magneto-rheological fluid |
| JP2018529704A JP6619099B2 (en) | 2015-08-28 | 2016-08-25 | Nanomagnetic rheological fluid and manufacturing equipment and method thereof |
| PCT/CN2016/096635 WO2017036337A1 (en) | 2015-08-28 | 2016-08-25 | Nano magneto-rheological fluid and preparation method and device thereof |
| CN201680050121.4A CN108352235B (en) | 2015-08-28 | 2016-08-25 | Nano magnetic rheological fluid and preparation equipment and method thereof |
| US15/807,146 US10896776B2 (en) | 2015-08-28 | 2017-11-08 | Nano magneto-rheological fluid and preparation method and device thereof |
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| CN108352235A (en) * | 2015-08-28 | 2018-07-31 | 湖南博海新材料股份有限公司 | Nanometer magneto-rheological fluid and its Preparation equipment and method |
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| CN106910587B (en) * | 2017-03-16 | 2019-02-01 | 黑龙江省科学院高技术研究院 | A kind of preparation method of loudspeaker magnetic fluid |
| CN108831663A (en) * | 2018-06-06 | 2018-11-16 | 冀中能源集团有限责任公司 | A kind of preparation method and its device of ore dressing magnetic fluid |
| CN110534329B (en) * | 2019-08-26 | 2022-04-19 | 深圳大学 | Preparation method of iron-nickel alloy magnetic fluid |
| CN112863803A (en) * | 2019-11-28 | 2021-05-28 | 台北科技大学 | Magnetorheological fluid and manufacturing method thereof |
| CN113205954A (en) * | 2021-04-20 | 2021-08-03 | 袁明凯 | Device for preparing nano magnetorheological fluid |
| CN117219391B (en) * | 2023-11-09 | 2024-01-23 | 深圳博海新材料技术有限公司 | Magnetorheological fluid with prolonged service life, preparation method thereof and magnetorheological damper |
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