CN104479814A - Preparation method of magneto-rheological grease - Google Patents
Preparation method of magneto-rheological grease Download PDFInfo
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Abstract
The invention provides a preparation method of magneto-rheological grease. The preparation methodis characterized by comprising the following steps: base oil is divided into three parts, the first part and the second part have the same weight, and the third part is 50 g more than the first part; the first part is taken and heated to 60 DEG C, fatty acid is added, the mixture is heated continuously to 80-100 DEG C, a lithium hydroxide aqueous solution is added, and the mixture is saponified for 1-3 h; the mixture is heated to 120-130 DEGC, the temperature is kept and dehydration is performed for 30 min; the second part of base oil and magnetic response particles are mixed and added to the mixture, the mixture is heated to the highest refining temperature of 190-220 DEG C, and heat is preserved for 5-7 min; and then the third part of base oil is added, and the mixture is cooled and ground to prepare the grease. The magneto-rheological fluid with high consistency has good wear resistance, lubrication, oxidation resistance, sealing performance and the like, and rheological characteristics of the fluid can be controlled through an external magnetic field, so that mechanical properties of equipment are improved, and the magneto-rheological grease can be applied to various equipment including a brake, a piston, a clutch, a buffer, sports equipment, a toy, a controllable composite structure and a structure component.
Description
Technical field
The present invention relates to a kind of preparation method of magnetorheological grease.
Background technology
Current, magnetic converting technique is applied to mechanical system, to control vibrations or noise.Magneto-rheological fluid viscosity is usually lower, magnetorheological devices must use precise part, expensive sealing, expensive bearing for this reason, this makes the use cost of magnetorheological devices greatly increase, and is difficult to extensively promote the use of, can only the higher specific occasion of application requiring.Therefore, need a kind of magnetic flow liquid of high-consistency, to avoid using specific installation to make magnetic flow liquid effectively keep in a device.Magnetorheological grease is exactly so a kind of magnetic flow liquid of high-consistency, and it has well wear-resistant, lubrication, anti-oxidant and sealing property etc., and controls its rheologic behavio(u)r by externally-applied magnetic field, thus improves the mechanical property of equipment.
The preparation method of traditional magnetorheological grease is the method directly adding the sub-homogenizing of magnetic response in finished product lubricating grease or base fat, as CN100437843C discloses " magnetorheological grease composition ", CN1414075A discloses " stability magnetorheological grease and preparation method thereof ", the magnetorheological grease denseness obtained is relatively low, mobility is better, but Adhering capacity is weak, sedimentation stability is poor, magnetic response easily produces sedimentation, its maximum centrifugal rate of descent, up to 28.9%, finally causes rheomagnetic to lose efficacy.
Summary of the invention
The present invention proposes a kind of magnetorheological grease new preparation process, is intended to ensure, on the basis of mobility, to improve the sedimentation stability of magnetorheological grease.
The object of the invention is to be realized by following measures:
A kind of magnetorheological grease preparation method, it is characterized in that: base oil is divided into 3 parts, the 1st part is identical with the 2nd part of weight, and the 3rd part than 50g more than the 1st part; Get the 1st part and be warming up to 60 DEG C, add lipid acid, continue to be warming up to 80 DEG C ~ 100 DEG C, add lithium hydroxide aqueous solution, saponification 1 ~ 3h; Be warming up to 120 DEG C ~ 130 DEG C, keep this temperature dehydration 30min; Add after 2nd part of base oil and magneticstrain mix particles, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, insulation 5min ~ 7min; Directly add the 3rd part of base oil, after cooling, grinding is obtained.In high temperature puffing process, magnetic response fully mixes with viscosifying agent (fatty acid lithium) and is disperseed very well in the liquid phase, thus denseness is comparatively greatly, Adhering capacity and sedimentation stability better.
Above-mentioned lipid acid is one or more in stearic acid, oleic acid, synthetic fatty acid or ten dihydroxystearic acids.
In order to improve dropping point, the heat embrittlement tendency of magnetorheological grease and divide wet goods performance, recombiner can also be added at cooling stages, as boric acid, hexanodioic acid and sebacic acid etc.
Preferably, above-mentioned saponification time is 1.5h ~ 2h, and reactant fully contacts, and the denseness of obtained magnetorheological grease is increasing, and dropping point also increases, and sedimentation stability is also better.Meanwhile, energy consumption is low, reduces costs.
Preferably, the highest above-mentioned refining temperature reaches 190 DEG C, keep 5min, oil soap mixture reaches molten state, now soap fiber is in molten state, under molten state, oil, soap, magnetic response are formed and keep collosol state, and the cone penetration of the magnetorheological grease of preparation is less, dropping point is higher, sedimentation stability is better.Prevent base oil vaporization losses from increasing, degree of oxidation increases simultaneously.
Preferably, above-mentioned cooling adopts water-bath cooling, and the soap fiber of generation is longer, and thickening ability is relatively strong, and the ability of parcel absorption carbonyl iron dust is comparatively strong, and cone penetration is less, and sedimentation stability is better.
No matter at null field or under having field condition, the flow phenomenon of magnetorheological grease is similar to the non-Bingham fluid of plasticity type, and its apparent viscosity η reduces with the increase of shearing rate γ, and shear-stress τ increases with the increase of shearing rate γ.The rheological property impact of the highest refining temperature on magnetorheological grease is relatively little.When shearing rate γ is larger, reinforced opportunity and the type of cooling affect larger on the rheological property of magnetorheological grease.The sample that process of cooling adds carbonyl iron dust and rapid cooling mode is having easy appearance under field, shear conditions to divide a grease phenomenon, their shear-stress τ
msuddenly can decline, then slowly recover.The sample that saponification process or dilution add magnetic response and slow cooling mode then shows well.Occur that the reason of this phenomenon is by analysis: the mode adding carbonyl iron dust fast when cooling and cooling affects the growth of soap fiber, the ability of soap fibre-coated magnetic response is more weak, having under field, shear conditions, the sub magnetic field force owing to being subject to of magnetic response is greater than soap fibers adsorption power with shearing centrifugal force, and is separated.
Above-mentioned base oil can be the conventional grease base oils such as mineral oil, paraffin oils, naphthenic oil or synthetic hydrocarbon oil; Base oil can be any mixture of these base oils.Preferred base oil is non-volatile nonpolar, and not containing any a large amount of water.The common content of base oil of the present invention is about 20% ~ about 80%, is preferably about 45% ~ 75%.Thickening material can be precipitated silica, Fumed silica, polyureas, organic clay, metallic soap or metal soap complex etc.These things can commercially buy or adopt method well-known in the art to prepare.The content of viscosifying agent is generally 7% ~ 15%, the content about 5% ~ 50% of magnetic-responsive particles, is preferably 15% ~ 35%.
The form of magnetic-responsive particles of the present invention normally metal powder, the method preparation that its available those of ordinary skill in the art know.Prepare metal powder typical method and comprise water atomization, metal oxide back method, grinding or friction, electrolyte deposition, metal-carbonyl decomposition, rapid solidification or smelting process.Particle can be that spherical or spherical change case is as irregular shaping particle or ellipsoid shaped particle.Adopt and also can play to the method for modifying of magnetic-responsive particles the effect reducing sedimentation.
Magnetorheological grease can also comprise other component especially antioxidant, lubricant and viscosity modifier.Such optional components is that those of ordinary skill in the art know.The example of antioxidant comprises especially metal and nonmetal dithiophosphates, hindered phenol, aromatic amine and phenol red etc.The example of lubricant comprises organic aliphatic acid, fatty acid amine, lard, high molecular organophosphorus and phosphoric acid ester, and the example of viscosity modifier comprises polymkeric substance and multipolymer, methacrylic ester, diene (hydrocarbon) or the alkylating vinylbenzene of alkene.Use these components in a particular application that by according to magnetorheological grease composition should be used for determine.
Beneficial effect
1. magnetorheological grease is made up of the magnetic-responsive particles, base oil, viscosifying agent, additive etc. of micron-scale, and under magnetic field exists, magnetic-responsive particles is polarized, forms orderly particle chain or particle microfilament.Particle chain adds the apparent viscosity (resistance to flow) of fluid, causes defining the solid matter with yielding stress.After magnetic field is removed, particle returns state of disarray, and it can reduce the viscosity of magnetorheological grease.And this performance of magnetorheological grease can change by continuous reversible with magnetic field is stepless.Magnetorheological grease, in response to magnetic field, demonstrates controllable behavior.But many magnetorheological materials cause particle precipitation due to the gravity that the non-uniform Distribution of particle is undue, affect the magnetorheological activity of material.Contriver finds, in magnetorheological materials, gravity causes the reason one of particle precipitation to be that difference between the proportion of magnetic particle and carrying object proportion is very large, causes particle precipitation rapidly in magnetorheological materials; Two is to-and-fro movements in use or high speed rotating causes.Current, magnetic converting technique is applied to mechanical system to control vibrations or noise.Magneto-rheological fluid viscosity is usually lower, magnetorheological devices must use precise part, expensive sealing, expensive bearing for this reason, this makes the use cost of magnetorheological devices greatly increase, and is difficult to extensively promote the use of, can only the higher specific occasion of application requiring.Therefore, need a kind of magnetic flow liquid of high-consistency, to avoid using specific installation to make magnetic flow liquid effectively keep in a device.Magnetorheological grease of the present invention is exactly so a kind of magnetic flow liquid of high-consistency, and it has well wear-resistant, lubrication, anti-oxidant and sealing property etc., and controls its rheologic behavio(u)r by externally-applied magnetic field, thus improves the mechanical property of equipment.The present invention can comprise in stopper, piston, clutch coupling, snubber, sports equipment, toy, controllable composite structure and construction package at much equipment and using.Magnetorheological grease great majority of the present invention are applied to the occasion needing to have high yielding stress and the low cost magnetorheological composition without sedimentation.Such as, magnetorheological grease of the present invention can be applicable to need in the earthquake vibroshock of permanent stability, or the wind resistance deoscillator of bridge is medium.
2, the present invention mainly provides a kind of preparation method of magnetorheological grease, compares and can obtain good sedimentation stability with existing method under the condition of less viscosifying agent; In puffing process, add magnetic-responsive particles, make it oil, soap, magnetic-responsive particles therewith and formed and keep collosol state, be scattered in wherein preferably.
3. the magnetorheological grease that prepared by the present invention mainly contains following advantage compared with additive method:
(1) conventionally obtained magnetorheological grease denseness is relatively low, and mobility is better, but Adhering capacity is more weak, and sedimentation stability is poor.Mainly disperse unequal reason owing to stirring the magnetic response such as homogenizing and carbonyl iron dust particle absorption.The present invention adds magnetic-responsive particles in preparation process to be made it to immerse in fibrous texture, and improves the sedimentation stability of magnetorheological grease.
(2) the sample null field of optimised process or the apparent viscosity under having field condition and shear-stress is tested all larger.
(3) when magneticstrength is 196.0mT, the shear-stress that traditional method obtains sample with the variation tendency of shearing rate is: first increase with shearing rate and increase, after decline suddenly when certain value, then recover gradually again.Significantly point oily phenomenon is shown in experimentation.The sample of the inventive method then shows well.
(4) the magnetorheological grease consistency range that can prepare of present method is wide, expands the controlled range of magnetorheological grease.
Accompanying drawing explanation
Fig. 1 magnetorheological grease preparation technology of the present invention schema
Fig. 2 embodiment 1 obtains magnetorheological grease performance, and (A is the different sedimentation rate of saponification time magnetorheological grease and the relation of time; B is the variation tendency (196.0mT) of different saponification time magnetorheological grease apparent viscosity η with shearing rate γ; The shear-stress τ of different saponification time magnetorheological grease
mvariation tendency (196.0mT) with shearing rate γ)
Fig. 3 embodiment 2 obtains magnetorheological grease performance, and (A is the sedimentation rate of magnetorheological grease and the relation of time that difference adds iron opportunity; B is the variation tendency (196.0mT) of magnetorheological grease apparent viscosity η with shearing rate γ that difference adds iron opportunity; C is the variation tendency (196.0mT) of shear-stress τ M with shearing rate γ that difference adds the magnetorheological grease on iron opportunity)
Fig. 4 embodiment 3 obtains magnetorheological grease performance, and (A is the highest different sedimentation rate of refining temperature magnetorheological grease and the relation of time; B is the variation tendency (196.0mT) of magnetorheological grease apparent viscosity η with shearing rate γ of the highest different refining temperature; C is the shear-stress τ of the magnetorheological grease of the highest different refining temperature
mvariation tendency (196.0mT) with shearing rate γ)
Fig. 5 embodiment 4 obtains magnetorheological grease performance, and (A is the sedimentation rate of the magnetorheological grease of the different type of cooling and the relation of time; B is the variation tendency (196.0mT) of magnetorheological grease apparent viscosity η with shearing rate γ of the different type of cooling; C is the variation tendency (196.0mT) of magnetorheological grease shear-stress τ M with shearing rate γ of the different type of cooling)
Fig. 6 embodiment 5 obtains magnetorheological grease performance, and (A is magnetorheological grease centrifugation time and rate of descent relation; B is the variation tendency (196.0mT) of sample η with γ; C is the variation tendency (196.0mT) of sample τ M with γ)
The different base oil of Fig. 7 embodiment 5 obtains magnetorheological grease performance, and (A is the variation tendency (196.0mT) of magnetorheological grease η with γ of different base oil; B is the variation tendency (196.0mT) of different base oil magnetorheological grease τ M with γ)
Embodiment
Mode below by embodiment further illustrates the present invention, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
This routine magnetorheological grease contains carbonyl iron dust 20%, soap content (lithium 12-hydroxy stearate) 7%, base oil (methyl-silicone oil) 73%.
Preparation technology: get 1 part of base oil 108.0g and be warming up to 60 DEG C, add 29.9g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 4.7g lithium hydroxide, saponification 1h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 104.6g, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, add DT-5 carbonyl iron dust 100.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.
Above-mentioned steps is constant, and preparation saponification time is respectively 1.5 ~ 2h, the example of 2 ~ 3h.
Embodiment 2
This routine magnetorheological grease contains carbonyl iron dust 20%, soap content (lithium 12-hydroxy stearate) 7%, base oil (methyl-silicone oil) 73%.
Preparation technology: get 1 part of base oil 107.5g and be warming up to 60 DEG C, add 30.2g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 4.8g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 106.6g, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, add DT-5 carbonyl iron dust 101.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.
Above-mentioned steps is constant, and preparation saponification stage and cooling stages add the example of carbonyl iron dust.
Embodiment 3
This routine magnetorheological grease contains carbonyl iron dust 20%, soap content (lithium 12-hydroxy stearate) 7%, base oil (methyl-silicone oil) 73%.
Preparation technology: get 1 part of base oil 108.5g and be warming up to 60 DEG C, add 29.8g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 4.7g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 107.8g, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, add DT-5 carbonyl iron dust 100.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.
Above-mentioned steps is constant, prepares the example of the highest refining temperature 200 DEG C ~ 210 DEG C and 210 DEG C ~ 220 DEG C.
Embodiment 4
This routine magnetorheological grease contains carbonyl iron dust 20%, soap content (lithium 12-hydroxy stearate) 7%, base oil (methyl-silicone oil) 73%.
Preparation technology: get 1 part of base oil 108.6g and be warming up to 60 DEG C, add 29.8g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 4.7g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 107.8g, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, add DT-5 carbonyl iron dust 100.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.
Above-mentioned steps is constant, prepares naturally cooling and the water-cooled example of ice.
Embodiment 5
This example first prepares soap content (lithium 12-hydroxy stearate) 7% according to CN1414075A method, base oil (methyl-silicone oil) 73%.Basic fat, then by basic fat heating and melting to molten state, keep temperature 190 DEG C ~ 220 DEG C add DT-5 carbonyl iron dust 20%, stir, cool.
New preparation process: get 1 part of base oil 108.0g and be warming up to 60 DEG C, add 29.9g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 4.7g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 104.6g, be warming up to the highest refining temperature 190 DEG C ~ 200 DEG C, add DT-5 carbonyl iron dust 100.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.Product performance are shown in Fig. 6.
Better example is prepared according to this condition:
Preparation method: (1) is got 1 part of 150BS base oil 102.0g and is warming up to 60 DEG C, adds 39.9g ten dihydroxystearic acid, continues to be warming up to 80 DEG C ~ 100 DEG C, adds the saturated aqueous solution containing 5.8g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 102.2g, be warming up to the highest refining temperature 190 DEG C ~ 200 DEG C, add DT-5 carbonyl iron dust 101.7g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.(2) get 1 part of methyl-silicone oil 85.4g and be warming up to 60 DEG C, add 39.9g ten dihydroxystearic acid, continue to be warming up to 80 DEG C ~ 100 DEG C, add the saturated aqueous solution containing 5.8g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 84.6g, be warming up to the highest refining temperature 190 DEG C ~ 200 DEG C, add DT-5 carbonyl iron dust 150.3g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.(3) get 1 part of PAO base oil 71.6g and be warming up to 60 DEG C, add 30.7g ten dihydroxystearic acid, continue to be warming up to 80 DEG C ~ 100 DEG C, add the saturated aqueous solution containing 4.3g lithium hydroxide, saponification 1.5 ~ 2h; Be warming up to 120 DEG C ~ 130 DEG C, dehydration 30min; Add the 2nd part of base oil 71.6g, be warming up to the highest refining temperature 190 DEG C ~ 200 DEG C, add DT-5 carbonyl iron dust 200g simultaneously, insulation 5min ~ 7min; 3rd part of base oil, than other 50g more than two parts, makes cooling oil; The obtained finished product of grinding after water-bath cooling.Product performance are shown in Fig. 7.
The denseness of magnetorheological grease is determined jointly by carbonyl iron dust content, base oil viscosity and saponified matter content.Saponified matter content increases, and denseness increases; Base oil viscosity increases, and denseness increases; Carbonyl iron dust content increases, and denseness increases, and shear-stress increases simultaneously.
Preparation technology is on the impact of magnetorheological grease physicochemical property
Note: sedimentation rate is at 40 DEG C, under the rotating speed of 10000rpm, centrifugal 30min, supernatant liquor accounts for the per-cent of magnetorheological grease total amount.Other step and parameter are optimum condition.
Claims (6)
1. a magnetorheological grease preparation method, is characterized in that: base oil is divided into 3 parts, and the 1st part identical with the 2nd part of weight, and the 3rd part than 50g more than the 1st part; Get the 1st part and be warming up to 60 DEG C, add lipid acid, continue to be warming up to 80 DEG C ~ 100 DEG C, add lithium hydroxide aqueous solution, saponification 1 ~ 3h; Be warming up to 120 DEG C ~ 130 DEG C, keep temperature dehydration 30min; Add after 2nd part of base oil and magnetic-responsive particles mixing, be warming up to the highest refining temperature 190 DEG C ~ 220 DEG C, insulation 5min ~ 7min; Add the 3rd part of base oil, after cooling, grinding is obtained.
2. magnetorheological grease preparation method as claimed in claim 1, described lipid acid is one or more in stearic acid, oleic acid, synthetic fatty acid or ten dihydroxystearic acids.
3. magnetorheological grease preparation method as claimed in claim 1 or 2, can also add recombiner at cooling stages, described recombiner is that boric acid, hexanodioic acid are or/and sebacic acid.
4. the magnetorheological grease preparation method as described in claim 1,2 or 3, described saponification time is 1.5h ~ 2h.
5. the magnetorheological grease preparation method as described in claim 1,2 or 3, the highest described refining temperature reaches 190 DEG C, keeps 5min.
6. the magnetorheological grease preparation method as described in claim 1,2 or 3, described cooling adopts water-bath cooling.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108467763A (en) * | 2018-01-23 | 2018-08-31 | 江苏大学 | A kind of preparation method of graphene-containing lithium base grease |
| CN110041987A (en) * | 2018-01-16 | 2019-07-23 | 中国人民解放军陆军勤务学院 | A kind of stable type, resistance to oxidation, high magnetic rheology effect magnetorheological grease |
| CN115433625A (en) * | 2022-09-30 | 2022-12-06 | 北京金茂人居环境科技有限公司 | Composite lithium-based magnetorheological grease and preparation method thereof |
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2014
- 2014-12-23 CN CN201410810168.9A patent/CN104479814A/en active Pending
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| 王正良: "滚动轴承的磁性流体润滑和密封研究", 《摩擦学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110041987A (en) * | 2018-01-16 | 2019-07-23 | 中国人民解放军陆军勤务学院 | A kind of stable type, resistance to oxidation, high magnetic rheology effect magnetorheological grease |
| CN108467763A (en) * | 2018-01-23 | 2018-08-31 | 江苏大学 | A kind of preparation method of graphene-containing lithium base grease |
| CN115433625A (en) * | 2022-09-30 | 2022-12-06 | 北京金茂人居环境科技有限公司 | Composite lithium-based magnetorheological grease and preparation method thereof |
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Effective date of abandoning: 20171208 |