CN104560301A - Mineral oil based magnetorheological fluid for high power transmission and preparation method thereof - Google Patents
Mineral oil based magnetorheological fluid for high power transmission and preparation method thereof Download PDFInfo
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- CN104560301A CN104560301A CN201410759564.3A CN201410759564A CN104560301A CN 104560301 A CN104560301 A CN 104560301A CN 201410759564 A CN201410759564 A CN 201410759564A CN 104560301 A CN104560301 A CN 104560301A
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Abstract
The invention discloses mineral oil based magnetorheological fluid for high power transmission. The mineral oil based magnetorheological fluid comprises the following components by mass percent: 60-80% of magnetic particles, 15-40% of carrier liquid and 2-5% of additives, wherein the magnetic particles are carbonyl iron powder particles and nano ferriferrous oxide particles; the carrier liquid is mineral oil; the additives comprise a surface active agent, a thixotropic agent, an antioxidant and an antiwear agent, meanwhile, the invention further provides a preparation method of the magnetorheological fluid, and the prepared magnetorheological fluid has excellent sedimentation stability, lower zero field viscosity, higher shear yield stress and long service life, and can meet the application requirements of high power transmission devices.
Description
Technical field
The present invention relates to a kind of magnetic flow liquid, specifically a kind of high-power transmission mineral oil based magnetic flow liquid and preparation method thereof, belongs to magnetic flow liquid technical field.
Background technology
Magnetic flow liquid is the liquid-solid two-phase intelligent material that a kind of rheological characteristics can control by externally-applied magnetic field and retrain, and is dispersed in primarily of micron-sized magnetic-particle and additive the suspension liquid formed in carrier fluid uniformly.This special suspension liquid is not when having externally-applied magnetic field, and its apparent viscosity is lower, shows as the liquid can free-pouring with Newtonian fuid characteristic; When there being externally-applied magnetic field, can there is violent change in the rheological characteristics of liquid in several millimeters, becomes the great class solid of viscosity, externally show certain yielding stress; Becoming again after removing magnetic field can free-pouring liquid, and the conversion between this solid-liquid occurred under additional the action of a magnetic field is reversible, rapidly, and the change of viscosity is continuous print.Therefore the characteristic of this uniqueness makes magnetic flow liquid be widely used in the fields such as aerospace, automotive industry, building trade, biologic medical, military affairs and national defence.
At present, have made some progress the investigation and application of magnetic flow liquid, but magnetic flow liquid also has some scabrous problems: sedimentation stability is poor, null field viscosity is large, shear yield stress is little, this has had a strong impact on its application in engineering machinery; Therefore, the practical application of over-all properties to magnetic flow liquid improving magnetic flow liquid is most important.
Summary of the invention
For above-mentioned prior art Problems existing, the invention provides a kind of high-power transmission mineral oil based magnetic flow liquid and preparation method thereof, magnetic flow liquid after preparation has excellent sedimentation stability, lower null field viscosity and higher shear yield stress, long service life, can meet the application requiring of severe duty drive.
To achieve these goals, the technical solution used in the present invention is: a kind of high-power transmission mineral oil based magnetic flow liquid,
Comprise the composition of following mass percent:
Magnetic-particle 60% ~ 80%;
Carrier fluid 15% ~ 40%;
Additive 2% ~ 5%;
Wherein, described magnetic-particle is carbonyl iron dust particle and nano ferriferrous oxide granule;
Described carrier fluid is mineral oil;
Described additive comprises tensio-active agent, thixotropic agent, antioxidant and anti-wear agent.
Described magnetic-particle is footpath grain is 2-4
μmcarbonyl iron dust particle and particle diameter be 20-40
nmferriferrous oxide particles.
Described nano ferriferrous oxide content is 4% ~ 6%.
Described carrier fluid is viscosity is that the mineral oil of 50cst ~ 100cst is as external phase.
Described tensio-active agent is any one or more than one the mixture in oleic acid, HT-610 Multi-functional dispersion anti-settling agent and Tween-80; Wherein, HT-610 Multi-functional dispersion anti-settling agent based on the extraordinary boundary material with multiple anchoring group, be aided with various different additive and be composited.
Described thixotropic agent is the mixture of any one or both in diatomite and organobentonite.
Described antioxidant is any one or more than one the mixture in nitrogen-containing heterocycle compound, nitrite and phenylformic acid.
Described anti-wear agent is the mixture of any one or both in silicon-dioxide and graphite.
Wherein, also comprise a kind of preparation method of high-power transmission mineral oil based magnetic flow liquid, comprise the following steps:
(be distributed to the 1 carbonyl iron dust uniform particles that a certain amount of acidifying is activated and be equipped with in the three-necked bottle of chemical plating fluid, and bubbling passes into nitrogen, keep reaction process ventilation, uniform stirring 2h under the condition of heating in water bath 65 DEG C; Wash after separating mixture, vacuum-drying under low pressure, obtain modified carbonyl ferrous powder granules;
(2 utilize coprecipitation method to obtain modified Nano ferriferrous oxide particles, concrete: by the FeC1 of certain mass
36H
2o and FeC1
24H
2o mixing ensures Fe in mixed solution
2+with Fe
3ratio is 1:1.5, and mixed solution is placed in four-hole boiling flask, high-speed stirring under the condition of heating in water bath 50 DEG C;
Dropwise dripping NaOH solution to reacting system PH value under passing into nitrogen protection is 10 ~ 11, adjusts the temperature to 70 DEG C, slaking 1h; By solution high speed centrifugation after slaking, then wash, wash away the unreacted foreign ion of particle surface, remove supernatant liquid, obtain Fe
3o
4colloidal solution;
Appropriate silane coupling agent is dissolved in a certain proportion of dehydrated alcohol and water, makes it be slightly acidic with the pH value of dilute hydrochloric acid regulator solution, treat that silane coupling agent is hydrolyzed for some time and Fe
3o
4colloidal solution mixes and vigorous stirring mutually, and be warming up to 70 DEG C of continuation vigorous stirring and react for some time, reaction terminates rear high speed centrifugation and repetitive scrubbing, vacuum-drying under low pressure, obtains the nanometer Fe of surface modification after grinding levigate sieving
3o
4particle;
(a certain proportion of additive is dissolved in mineral oil by 3, and uniform stirring 2h under the condition of heating in water bath 50 DEG C, obtains composite carrier fluid;
The modified carbonyl ferrous powder granules that (4 by step 1) and step 2) obtains and modified Nano ferriferrous oxide particles join in the composite carrier fluid of the 3rd step, homogenous disperse machine high speed dispersion under the condition that heating in water bath is 50 DEG C;
(said mixture is placed in ball mill by 5, with rotating speed 250rmin
-1ball milling 8 ~ 10 hours, obtains magnetic flow liquid finished product.
Chemical plating fluid in step 1) is the reaction solution containing cobalt element.
Compare with formula with existing preparation method, the present invention has following characteristics:
1, the base load liquid of current oil base magnetic flow liquid is mainly based on silicone oil.Because the additive of many improving SNR is not compatible with silicone oil, the magnetic flow liquid therefore prepared has larger viscosity, is easy to caking and precipitation, can not meets the application requiring of high-power transmission magnetic flow liquid.And high-power transmission mineral oil based magnetic flow liquid of the present invention, select viscosity low and the mineral oil base oil with good fluidity is carrier fluid, this base load liquid viscosity when room temperature (25 DEG C) is 50cst ~ 100cst, with multiple additives, there is excellent compatibility, the high-power transmission magnetic flow liquid prepared with it has lower null field viscosity, and (25 DEG C are operated in shearing rate when being 50 ~ 310s-1,0.48Pas ~ 0.93Pas) and good low temperature properties, be applicable to recycling of high-power transmission device;
2, the present invention selects the carbonyl iron dust particle of high permeability and low-coercivity to be main disperse phase, and nano ferriferrous oxide granule is auxiliary disperse phase.Wherein the add-on of nano ferriferrous oxide is 4% ~ 6% of magnetic flow liquid quality, this suitable add-on can improve sedimentation stability and the shear yield stress of liquid, when without externally-applied magnetic field, nano particle and base fluid can form the carrier fluid of magnetic flow liquid jointly, increase the density of carrier fluid, thus the sedimentation that the density difference reducing particle and carrier fluid causes, in addition, nano particle can do random pedesis in carrier fluid, continuous collision carbonyl iron dust particle, play the effect stoping particles sink, therefore suitable nano particle improves the sedimentation stability of magnetic flow liquid, when there being the action of a magnetic field, carbonyl iron dust particle alignment chaining, appropriate nano ferriferrous oxide granule is filled in the gap of carbonyl iron dust particle chain, thus forms the particle chain that can bear larger shearing stress, improves shear yield stress.
3, high-power transmission mineral oil based magnetic flow liquid of the present invention has carried out surface coating modification to the magnetic-particle selected, and nanometer cobalt particle is coated on the surface of carbonyl iron dust particle, improves shear yield stress; Nano ferriferrous oxide granule is coated by silane surface active agent, improves oxidation-resistance.
4, the present invention select in oleic acid, HT-610 and Tween-80 any one or multiple as tensio-active agent.A kind of oligopolymer having special molecular structure that tensio-active agent is made up of hydrophilic group and oleophilic group, science adds proper amount of surfactant, hydrophilic group is made to be adsorbed on the surface of magnetic-particle, and the oleophilic group of one end is diffused in the middle of the carrier fluid of low-to-moderate polarity, the volume of such increase particle, reduce they attract each other collision chance, and can be formed sterically hindered in carrier fluid inside, form an interactional three-dimensional net structure, thus the density difference reduced due to particle and carrier fluid and the particles settling that causes, improve the sedimentation stability of magnetic flow liquid.
5, the present invention select in diatomite and organobentonite any one or multiple as thixotropic agent, select in nitrogen-containing heterocycle compound, nitrite and phenylformic acid any one or multiple as antioxidant, select in silicon-dioxide and graphite any one or multiple as anti-wear agent, magnetic flow liquid is made to have good oxidation-resistance and resistance to abrasion, long service life.
Accompanying drawing explanation
Fig. 1 be coated after the SEM photo of magnetic-particle;
Fig. 2 is the magnetic flow liquid null field viscogram of preparation;
Fig. 3 is the magnetorheological fluid sedimentation stability diagram of preparation;
Fig. 4 is the shear yield stress figure of the magnetic flow liquid of preparation.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
A kind of high-power transmission mineral oil based magnetic flow liquid,
Comprise the composition of following mass percent:
Magnetic-particle 60% ~ 80%;
Carrier fluid 15% ~ 40%;
Additive 2% ~ 5%;
Wherein, described magnetic-particle is carbonyl iron dust particle and nano ferriferrous oxide granule;
Described carrier fluid is mineral oil;
Described additive comprises tensio-active agent, thixotropic agent, antioxidant and anti-wear agent.
Described magnetic-particle to be footpath grain the be carbonyl iron dust particle of 2-4 μm and particle diameter are the ferriferrous oxide particles of 20-40nm, they have high permeability and low-coercivity, stablizing than energy retention in wide temperature range, can ensure that magnetic flow liquid has longer working life and stability.
Wherein, described nano ferriferrous oxide content is 4% ~ 6%, and suitable add-on can improve sedimentation stability and the shear yield stress of liquid.
Described carrier fluid to be viscosity the be mineral oil of 50cst ~ 100cst, as external phase, can ensure that magnetic flow liquid has less null field viscosity.
Described tensio-active agent is any one or more than one the mixture in oleic acid, HT-610 Multi-functional dispersion anti-settling agent and Tween-80; Wherein, HT-610 Multi-functional dispersion anti-settling agent based on the extraordinary boundary material with multiple anchoring group, be aided with various different additive and be composited; Improve the sedimentation stability of magnetic flow liquid.
Described thixotropic agent is the mixture of any one or both in diatomite and organobentonite.Described antioxidant is any one or more than one the mixture in nitrogen-containing heterocycle compound, nitrite and phenylformic acid.Described anti-wear agent is the mixture of any one or both in silicon-dioxide and graphite, and the interpolation of mentioned component makes magnetic flow liquid have good oxidation-resistance and resistance to abrasion, long service life.
Further illustrate in conjunction with the embodiments
Embodiment 1
Preparation volume fraction is the high-power transmission mineral oil based magnetic flow liquid of 20%, and namely the massfraction of magnetic-particle is 67%, and preparation process is:
(1 200g carbonyl iron dust particle is carried out acidifying activation treatment after be distributed in the three-necked bottle that chemical plating fluid (reaction solution containing cobalt element) is housed, pass into nitrogen, keep ventilating in reaction process always, uniform stirring 2h under the condition that heating in water bath is 65 DEG C, after stirring terminates, separating mixture also washs, vacuum-drying under low pressure, obtains cobalt plating carbonyl iron dust particle;
(2 by the FeC1 of certain mass
36H
2o and FeC1
24H
2o mixing ensures Fe in mixed solution
2+with Fe
3+ratio is 1:1.5, gets 150
mlbe placed in four-hole boiling flask, high-speed stirring under the condition of heating in water bath 50 DEG C.Dropwise dripping NaOH solution to reacting system PH value under passing into nitrogen protection is 10 ~ 11, adjusts the temperature to 70 DEG C, slaking 1
h, by solution high speed centrifugation after slaking, then wash, wash away the unreacted foreign ion of particle surface, remove supernatant liquid, obtain Fe
3o
4colloidal solution.Appropriate silane coupling agent is dissolved in a certain proportion of dehydrated alcohol and water, makes it be slightly acidic with the pH value of dilute hydrochloric acid regulator solution, treats that silane coupling agent is hydrolyzed for some time and Fe
3o
4colloidal solution mixes and vigorous stirring mutually, and be warming up to 70 DEG C of continuation vigorous stirring and react for some time, reaction terminates rear high speed centrifugation and repetitive scrubbing, vacuum-drying under low pressure, obtains the nanometer Fe of surface modification after grinding levigate sieving
3o
4particle;
(3, by a certain proportion of additive, are specially 1.7
ghT-610,1
gdiatomite, 1.5
gorganobentonite, 1
gphenylformic acid, 1
gsilicon-dioxide and 1.5
ggraphite, be added to 100 successively
gin mineral oil, uniform stirring 2 under the condition of heating in water bath 50 DEG C
h, obtain composite carrier fluid;
(the modified Nano ferriferrous oxide particles (getting 15g) in the cobalt plating carbonyl iron dust of the first step and second step is mixed to join in the composite carrier fluid of the 3rd step by 4, homogenous disperse machine high speed dispersion under the condition that heating in water bath is 50 DEG C;
(said mixture is placed in ball mill by 5, with rotating speed 250 rmin
-1ball milling 10 hours, obtains magnetic flow liquid finished product.
Embodiment 2
Preparation volume fraction is the high-power transmission mineral oil based magnetic flow liquid of 25%, and namely the massfraction of magnetic-particle is 75%, and preparation process is:
(1 by 305
gcarbonyl iron dust particle is distributed to after carrying out acidifying activation treatment in the three-necked bottle that chemical plating fluid (reaction solution containing cobalt element) is housed, and passes into nitrogen, keeps ventilating in reaction process always, uniform stirring 2 under the condition that heating in water bath is 70 DEG C
h; After stirring terminates, separating mixture also washs, vacuum-drying under low pressure, obtains cobalt plating carbonyl iron dust particle;
(2 obtain the nanometer Fe of modification according to the step in embodiment 1
3o
4particle;
(3, by a certain proportion of additive, are specially 2.6
ghT-610,1.4
gdiatomite, 2.3
gorganobentonite, 1.8
gphenylformic acid, 1.6
gsilicon-dioxide and 1.5
ggraphite, be added to 100 successively
gin mineral oil, uniform stirring 2 under the condition of heating in water bath 50 DEG C
h, obtain composite carrier fluid;
(the modified Nano ferriferrous oxide particles (getting 20g) in the cobalt plating carbonyl iron dust of the first step and second step is mixed to join in the composite carrier fluid of the 3rd step by 4, homogenous disperse machine high speed dispersion under the condition that heating in water bath is 50 DEG C;
(said mixture is placed in ball mill by 5, with rotating speed 250 rmin
-1ball milling 10 hours, obtains magnetic flow liquid finished product
Embodiment 3
Preparation volume fraction is the high-power transmission mineral oil based magnetic flow liquid of 30%, and namely the massfraction of magnetic-particle is 80%, and preparation process is:
(1 by 400
gcarbonyl iron dust particle is distributed to after carrying out acidifying activation treatment in the three-necked bottle that chemical plating fluid (reaction solution containing cobalt element) is housed, and passes into nitrogen, keeps ventilating in reaction process always, uniform stirring 2 under the condition that heating in water bath is 70 DEG C
h; After stirring terminates, separating mixture also washs, vacuum-drying under low pressure, obtains cobalt plating carbonyl iron dust particle;
(2 obtain the nanometer Fe of modification according to the step in embodiment 1
3o
4particle;
(3, by a certain proportion of additive, are specially 3.5
ghT-610,2.2
gdiatomite, 3
gorganobentonite, 1.8
gphenylformic acid, 2
gsilicon-dioxide and 2
ggraphite, be added to 100 successively
gin mineral oil, uniform stirring 2 under the condition of heating in water bath 50 DEG C
h, obtain composite carrier fluid;
(the modified Nano ferriferrous oxide particles (getting 24g) in the cobalt plating carbonyl iron dust of the first step and second step is mixed to join in the composite carrier fluid of the 3rd step by 4, homogenous disperse machine high speed dispersion under the condition that heating in water bath is 50 DEG C;
(said mixture is placed in ball mill by 5, with rotating speed 250 rmin
-1ball milling 10 hours, obtains magnetic flow liquid finished product.
Further illustrate by reference to the accompanying drawings, wherein add contrast sample 1: publication number is that CN103525505A mono-kind can strengthen the carbonyl iron dust of magnetic rheology effect and the magnetic flow liquid of preparation thereof, contrast sample 2: publication number is CN101457172A stabilizing type magnetic rheological fluid, contrast sample 3: publication number is magnetic flow liquid of CN103897789A polymer composite magnetic powder and preparation method thereof, contrast sample 4: silicone oil based magnetic rheologic liquid that publication number CN1959872A mono-kind is stable and preparation method thereof.
As shown in Figure 1, less in figure particle is modified Nano ferriferrous oxide particles; The particle of larger sub-circular is modified carbonyl ferrous powder granules, can see that there is the fibrous coating layer of one deck on its surface, and this adds the coated result of additive.Be be connected together by this fibrous structural chain between particle after adding additive, thus avoid the direct contact between particle, improve sedimentation stability, reduce caking of reuniting, reduce null field viscosity.
Figure 2 shows that the relation curve of magnetic flow liquid null field viscosity and shearing rate; The null field viscosity of the magnetic flow liquid of the application presents the trend of reduction with the increase of shearing rate; Magnetic flow liquid null field viscosity prepared by the present invention is less than contrast sample 1 and contrast sample 2.
Figure 3 shows that the relation curve of magnetorheological fluid sedimentation speed relative to the time; The magnetorheological fluid sedimentation speed of preparation of the present invention is finally 8%, 8.3% and 10% having left standstill 20 days afterwards, and stability is better than contrast sample 1 and contrast sample 3, and to be better than the contrast sample 4(subsidence rate left standstill after 20 days be 12% ~ 18%), there is excellent stability.
Figure 4 shows that the relation curve of shear yield stress and magnetic induction density; Along with the increase of magnetic induction density, shear yield stress constantly increases, magnetic flow liquid prepared by the present invention is when magnetic induction density is 0.5T, shear yield stress is 27.5kPa, 30kPa and 34kPa, and numerical value is higher than contrast sample 2, and magnetic induction density is when being 0.7T, Shear Yield Stress of Magnetorheological Fluids prepared by the present invention is 55kPa, 57kPa and 60.8kPa, has high shear yield stress.
Claims (10)
1. a high-power transmission mineral oil based magnetic flow liquid, is characterized in that,
Comprise the composition of following mass percent:
Magnetic-particle 60% ~ 80%;
Carrier fluid 15% ~ 40%;
Additive 2% ~ 5%;
Wherein, described magnetic-particle is carbonyl iron dust particle and nano ferriferrous oxide granule;
Described carrier fluid is mineral oil;
Described additive comprises tensio-active agent, thixotropic agent, antioxidant and anti-wear agent.
2. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described magnetic-particle is footpath grain is 2-4
μmcarbonyl iron dust particle and particle diameter be the ferriferrous oxide particles of 20-40.
3. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, it is characterized in that, described nano ferriferrous oxide content is 4% ~ 6%.
4. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described carrier fluid is viscosity is that the mineral oil of 50cst ~ 100cst is as external phase.
5. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described tensio-active agent is any one or more than one the mixture in oleic acid, HT-610 Multi-functional dispersion anti-settling agent and Tween-80; Wherein, HT-610 Multi-functional dispersion anti-settling agent based on the extraordinary boundary material with multiple anchoring group, be aided with various different additive and be composited.
6. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described thixotropic agent is the mixture of any one or both in diatomite and organobentonite.
7. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described antioxidant is any one or more than one the mixture in nitrogen-containing heterocycle compound, nitrite and phenylformic acid.
8. a kind of high-power transmission mineral oil based magnetic flow liquid according to claim 1, is characterized in that, described anti-wear agent is the mixture of any one or both in silicon-dioxide and graphite.
9. a high-power transmission preparation method for mineral oil based magnetic flow liquid, is characterized in that, comprise the following steps:
(be distributed to the 1 carbonyl iron dust uniform particles that a certain amount of acidifying is activated and be equipped with in the three-necked bottle of chemical plating fluid, and bubbling passes into nitrogen, keep reaction process ventilation, uniform stirring 2h under the condition of heating in water bath 65 DEG C; Wash after separating mixture, vacuum-drying under low pressure, obtain modified carbonyl ferrous powder granules;
(2 utilize coprecipitation method to obtain modified Nano ferriferrous oxide particles, concrete: by the FeC1 of certain mass
36H
2o and FeC1
24H
2o mixing ensures Fe in mixed solution
2+with Fe
3ratio is 1:1.5, and mixed solution is placed in four-hole boiling flask, high-speed stirring under the condition of heating in water bath 50 DEG C;
Dropwise dripping NaOH solution to reacting system PH value under passing into nitrogen protection is 10 ~ 11, adjusts the temperature to 70 DEG C, slaking 1h; By solution high speed centrifugation after slaking, then wash, wash away the unreacted foreign ion of particle surface, remove supernatant liquid, obtain Fe
3o
4colloidal solution;
Appropriate silane coupling agent is dissolved in a certain proportion of dehydrated alcohol and water, makes it be slightly acidic with the pH value of dilute hydrochloric acid regulator solution, treat that silane coupling agent is hydrolyzed for some time and Fe
3o
4colloidal solution mixes and vigorous stirring mutually, and be warming up to 70 DEG C of continuation vigorous stirring and react for some time, reaction terminates rear high speed centrifugation and repetitive scrubbing, vacuum-drying under low pressure, obtains the nanometer Fe of surface modification after grinding levigate sieving
3o
4particle;
(a certain proportion of additive is dissolved in mineral oil by 3, and uniform stirring 2h under the condition of heating in water bath 50 DEG C, obtains composite carrier fluid;
The modified carbonyl ferrous powder granules that (4 by step 1) and step 2) obtains and modified Nano ferriferrous oxide particles join in the composite carrier fluid of the 3rd step, homogenous disperse machine high speed dispersion under the condition that heating in water bath is 50 DEG C;
(said mixture is placed in ball mill by 5, with rotating speed 250rmin
-1ball milling 8 ~ 10 hours, obtains magnetic flow liquid finished product.
10. a high-power transmission preparation method for mineral oil based magnetic flow liquid, is characterized in that, the chemical plating fluid in step 1) is the reaction solution containing cobalt element.
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