CN1959872A - Stable silicone oil based magnetic rheologic liquid, and preparation method - Google Patents
Stable silicone oil based magnetic rheologic liquid, and preparation method Download PDFInfo
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Abstract
The magnetic rheologic liquid is composed of components: chelation type surfactant / carbonyl iron hull type magnetic compound particles, and silicone oil based compound assorted carrier liquid prepared from silicone oil and additive. The additive includes thixotropic agent, antioxidant, antiwear additive, and surfactant. The method for preparing the liquid includes steps: mixing round surfactant being added to silicone oil; next, adding antioxidant, thixotropic agent, and antiwear agent, then mixing them to obtain silicone oil based compound assorted carrier liquid; adding magnetic compound particles to the carrier liquid, and after procedures of mixing, ballmilling, and separating out friction balls, then sealing the liquid inside plastic bottle; stable silicone oil based magnetic rheologic liquid is obtained after series of procedure: placing the plastic bottle in magnetic field, taking out the liquid, and mixing etc. The liquid is applicable to damper, variator for cars etc.
Description
Technical field
The present invention relates to a kind of magnetic flow liquid and preparation method thereof, be specially a kind of stable silicone oil based magnetic rheologic liquid and preparation method thereof.
Technical background
Magnetic flow liquid is to be dispersed in the suspension that (claims base fluid usually) in the non magnetic liquid and form by magnetizable particles.It has a key property: under the situation about existing in magnetic field, the apparent viscosity of magnetic flow liquid is proportional to magnetic field intensity, and its intensity of variation can reach thousands of times, and this variation be fast, reversible, this characteristic is called magnetic rheology effect.Utilize this specific character can manufacture and design many new devices and new instrument, as MR damper, automobile magneto-rheological vibration damper, magnetorheological speed changer and magnetic rheological brake, magnetorheological sealing device, magnetorheological polishing instrument etc., its application prospect is huge.
Though the using value of magnetic flow liquid is revealed and confirmation, owing to the too poor application that has had a strong impact on it of its sedimentation stability.This is because be far longer than density as the liquid of continuous phase as the density of the magnetizable particles of magnetic flow liquid decentralized photo, and the base fluid of the magnetizable particles of decentralized photo and continuous phase is inconsistent.So the sedimentation stability difference of magnetic flow liquid just becomes its key in application factor in engineering of restriction.
In order to solve or improve the sedimentation stability problem of magnetic flow liquid, people have adopted many methods, as with the nanoscale magnetizable particles as decentralized photo, but the result to be magnetic rheology effect too little and reduced the engineering using value, and still can leave standstill postprecipitation and reunion for a long time; Patent CN1613919A discloses a kind of magnetic particle of close silicone oil polymer parcel and the preparation method of silicone oil based magnetic rheologic liquid thereof, and the magnetic flow liquid of this method preparation has improved non-oxidizability, but still has serious settlement issues; The hydroxyl effect with silane coupler and carbonyl iron particles particle surface that and for example proposes among the USP6824701 makes it to form the iron particles of silanization, though this method can be improved the sedimentation stability of magnetic flow liquid, preparation technology is complexity, and production cost is higher.The inventor of present patent application finds that under study for action the compound composite magnetic flow liquid of core-shell type magnetic particle of use high molecular polymer/carbonyl iron can shockingly improve the sedimentation stability and the magnetic rheology effect of magnetic flow liquid, and preparation technology is simple, and cost is low.
Summary of the invention
The object of the present invention is to provide a kind of stable silicone oil based magnetic rheologic liquid and preparation method thereof, overcome the shortcoming of poor, easy oxidation deterioration of magnetic metal particle suspension stability in silicone oil and caking, the magnetic flow liquid that is provided has good antioxygenic property, the friction resistant performance, and have good thixotropy.
A kind of silicone oil based magnetic rheologic liquid of the present invention is become by following components in mass portion array:
65～90 parts of magnetic particles, 10～35 parts of the composite carrier fluids of silicone oil base of silicone oil doping preparation;
Wherein said magnetic particle is chelate surfactant/carbonyl iron core-shell type magnetic compound particle, and its particle diameter is 1～100 micron;
Described additive comprises following component by magnetic flow liquid gross mass percentage:
Thixotropic agent: 0.05%～2%, composition is nanometer lithium magnesium silicate, polysaccharide, cellulose derivative or bentonite;
Antioxidant: 0.1%～1%, composition is natrium nitrosum, Sodium Benzoate or monoethanolamine phosphate;
Antiwear additive: 1%～3%, composition is graphite, nano alumina powder or nano-cerium oxide powder;
Surfactant: 0.1%～3%, composition is N-lauroyl ethylenediamine triacetic acid, neopelex, oleic acid or polyether-based benzene sulfonic acid sodium salt.
Described chelate surfactant/carbonyl iron core-shell type magnetic compound particle; be N-cetyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle; N-lauroyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle, N-docosyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle.
The preparation method of the composite carrier fluid of described magnetic flow liquid silicone oil base, its preparation process is:
Step 2, antioxidant is joined in the suspension that step 1 obtains by the amount of magnetic flow liquid gross mass 0.1%～1%, at room temperature mixed 2～4 hours, obtain suspension;
Step 3, thixotropic agent is joined in the suspension that step 2 obtains by the amount of magnetic flow liquid gross mass 0.05%～2%, at room temperature mixed 2～4 hours, obtain suspension;
Step 4, antiwear additive is added in the suspension that step 3 obtains by the amount of magnetic flow liquid gross mass 1%～3%, at room temperature mixed 2～4 hours, promptly make the composite carrier fluid of magnetic flow liquid silicone oil base.
Preparation method's step of described magnetic flow liquid is:
Step 2, the mixed material that step 1 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 200～300 rev/mins, ball milling 3～10 hours, isolate steel ball, obtain magnetic flow liquid, sealing is protected and is preserved in the plastic bottles of the capping of packing into.
The post-processing approach of silicone oil based magnetic rheologic liquid of the present invention: the above-mentioned silicone oil magnetic flow liquid that makes contained in plastic bottle seal, place the magnetic field of adjustable magnetic fields size, magnetic field intensity is adjusted to 100～400mT, magnetic flow liquid was taken out from magnetic field in per 10 days, stir after 5～20 minutes, contain in plastic bottle again and seal, place the magnetic field of adjustable magnetic fields size, magnetic field intensity is adjusted to 100～400mT, repeat aforesaid operations, after 20～60 days magnetic flow liquid is taken out from magnetic field, obtain stable silicone oil based magnetic rheologic liquid, sealing gets final product long preservation in the dry plastic bottle of packing into.
Silicone oil based magnetic rheologic liquid of the present invention adopts chelate surfactant/carbonyl iron core-shell type magnetic compound particle as magnetic particle, the good in oxidation resistance of particle, particularly the shell of compound particle has the organic molecule brush of close silicone oil, be dispersed in the silicone oil and can form pectinate texture, prevent the sedimentation and the reunion of particle effectively.Adopt the composite carrier fluid of silicone oil base simultaneously, the viscosity of carrier fluid has improved, and the thixotropic agent that helps improving in the sedimentation stability of magnetic flow liquid, particularly carrier fluid can form network configuration, can hinder the particle precipitation of decentralized photo.
Silicone oil based magnetic rheologic liquid of the present invention has significant magnetic rheology effect, excellent suspension stability, redispersibility and chemical stability, and characteristics such as low null field viscosity, can be widely used in Technique of Magnetorheological Finishing and make field such as magnetorheological device.
The method for preparing silicone oil based magnetic rheologic liquid provided by the invention, technology is fairly simple, and cost is lower.
Description of drawings
Fig. 1 is the relation curve of magnetic flow liquid null field viscosity of the present invention and shear rate.
Fig. 2 is the relation curve of magnetic flow liquid mangneto shear stress of the present invention and magnetic field intensity.
Fig. 3 leaves standstill volume fraction that the carrier fluid amount of separating out accounts for total amount curve over time for magnetic flow liquid of the present invention.
Curve among Fig. 3 is that 10 milliliters of magnetic flow liquids are added in the graduated test tube, leaves standstill for a long time, observes the carrier fluid amount of separating out relation curve over time.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Used chelate surfactant/carbonyl iron core-shell type magnetic compound particle (N-cetyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle, N-lauroyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle, N-docosyl ethylenediamine triacetic acid/carbonyl iron core-shell type magnetic compound particle), N-lauroyl ethylenediamine triacetic acid is that Tianyi Superfine Metal Powders Co., Ltd., Jiangsu produces among the embodiment, and other raw material is the commercial goods.
The present invention adopts the ARES 2000 senior expansion flow graphs of U.S. TA company to measure the rheological behavior of magnetic flow liquid.
The % amount that remarks additionally in the embodiment bracket is mass percent.
Embodiment 1:
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.5g (0.5%) antioxidant natrium nitrosum is joined in the mixture that step 1 obtains, at room temperature mixed 3 hours, mixture;
Step 3,0.5g (0.5%) thixotropic agent nanometer lithium magnesium silicate is joined in the mixture that step 2 obtains, at room temperature mixed 3 hours, mixture;
Step 4,2g (2%) antiwear additive graphite is joined in the mixture that step 3 obtains, at room temperature mixed 4 hours, promptly make silicone oil base compositional liquor carrier fluid;
Step 6, the mixed material that step 5 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 200 rev/mins, ball milling 10 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 400mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 5 minutes with glass bar after, 7 operations set by step again;
Step 9, after 20 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid null field viscosity with shear rate change (0.1～400s
-1) relation curve, see example 1 among Fig. 1.
(0～4000Gs) relation curve is seen example 1 among Fig. 2 with change of magnetic field strength to adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid mangneto shear stress.
The method of testing of the sedimentation stability of magnetic flow liquid is to add in the graduated graduated cylinder 10 milliliters of magnetic flow liquids and sealing, leave standstill, the record different time carrier fluid amount of separating out obtains magnetic flow liquid and leaves standstill the time dependent relation curve of volume fraction that the back carrier fluid amount of separating out accounts for total amount, sees example 1 among Fig. 3.
Embodiment 2
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.3g (0.3%) antioxidant Sodium Benzoate is joined in the mixture that step 1 obtains, at room temperature mixed 2 hours, mixture;
Step 3,0.7g (0.7%) thixotropic agent polysaccharide is joined in the mixture that step 2 obtains, at room temperature mixed 4 hours, mixture;
Step 4,1g (1%) antiwear additive nano alumina powder is joined in the mixture that step 3 obtains, at room temperature mixed 2 hours, promptly make the composite carrier fluid of silicone oil base;
Step 6, the mixed material that step 5 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 250 rev/mins, ball milling 6 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 300mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 10 minutes with glass bar after, 7 operations set by step again;
Step 9, after 30 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid null field viscosity with shear rate change (0.1～400s
-1) relation curve, see example 2 among Fig. 1.
(0～4000Gs) relation curve is seen example 2 among Fig. 2 with change of magnetic field strength to adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid mangneto shear stress.
Adopt embodiment 1 identical method to test the sedimentation stability of magnetic flow liquid, obtain magnetic flow liquid and leave standstill the time dependent relation curve of volume fraction that the back carrier fluid amount of separating out accounts for total amount, see example 2 among Fig. 3.
Embodiment 3
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.2g (0.2%) antioxidant monoethanolamine phosphate is joined in the mixture that step 1 obtains, at room temperature mixed 2 hours, mixture;
Step 3,0.3g (0.3%) thixotropic agent cellulose derivative is joined in the mixture of step 2, at room temperature mixed 2 hours, mixture;
Step 4,1.5g (1.5%) antiwear additive nano-cerium oxide powder is joined in the mixture that step 3 obtains, at room temperature mixed 3 hours, promptly make the composite carrier fluid of silicone oil base;
Step 6, the mixed material that step 5 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 250 rev/mins, ball milling 7 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 200mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 15 minutes with glass bar after, 7 operations set by step again;
Step 9, after 40 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid null field viscosity with shear rate change (0.1～400s
-1) relation curve, see example 3 among Fig. 1.
(0～4000Gs) relation curve is seen example 3 among Fig. 2 with change of magnetic field strength to adopt above-mentioned senior expansion flow graph to measure magnetic flow liquid mangneto shear stress.
Adopt embodiment 1 identical method to test the sedimentation stability of magnetic flow liquid, obtain magnetic flow liquid and leave standstill the time dependent relation curve of volume fraction that the back carrier fluid amount of separating out accounts for total amount, see example 3 among Fig. 3.
Embodiment 4
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.4g (0.4%) antioxidant natrium nitrosum is joined in the mixture of step 1, at room temperature mixed 3 hours, mixture;
Step 3,0.3g (0.3%) thixotropic agent bentonite is joined in the mixture that step 2 obtains, at room temperature mixed 2 hours, mixture;
Step 4,1.3g (1.3%) antiwear additive graphite is joined in the mixture that step 3 obtains, at room temperature mixed 3 hours, promptly make the composite carrier fluid of silicone oil base;
Step 6, the mixed material that step 5 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 300 rev/mins, ball milling 3 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 25mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 20 minutes with glass bar after, 7 operations set by step again;
Step 9, after 50 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Adopt embodiment 1 identical method to measure magnetic flow liquid null field viscosity with shear rate change (0.1～400s
-1) relation curve, see example 4 among Fig. 1.
(0～4000Gs) relation curve is seen example 4 among Fig. 2 with change of magnetic field strength to adopt embodiment 1 identical method to measure magnetic flow liquid mangneto shear stress.
Adopt embodiment 1 identical method to test the sedimentation stability of magnetic flow liquid, obtain magnetic flow liquid and leave standstill the time dependent relation curve of volume fraction that the back carrier fluid amount of separating out accounts for total amount, see example 4 among Fig. 3.
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.5g (0.5%) antioxidant Sodium Benzoate is joined in the mixture that step 1 obtains, at room temperature mixed 2 hours, mixture;
In step 3, the mixture, at room temperature mixed 4 hours, get mixture 1g (1%) thixotropic agent nanometer lithium magnesium silicate adding step 2;
Step 4,3g (3%) antiwear additive nano alumina powder is joined in the mixture that step 3 obtains, at room temperature mixed 2 hours, promptly make the composite carrier fluid of silicone oil base;
Step 6, the mixed material that step 6 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 250 rev/mins, ball milling 6 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 350mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 10 minutes with glass bar after, 7 operations set by step again;
Step 9, after 30 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Embodiment 6
Preparation 100g silicone oil based magnetic rheologic liquid, preparation process is:
Step 2,0.5g (0.5%) antioxidant monoethanolamine phosphate is joined in the mixture that step 1 obtains, at room temperature mixed 3 hours, mixture;
Step 3,1g (1%) thixotropic agent polysaccharide is joined in the mixture that step 2 obtains, at room temperature mixed 2 hours, mixture;
Step 4,2g (2%) antiwear additive nano-cerium oxide powder is joined in the mixture that step 3 obtains, at room temperature mixed 3 hours, promptly make the composite carrier fluid of silicone oil base;
Step 6, the mixed material that step 5 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 300 rev/mins, ball milling 3 hours, isolate steel ball, pack into magnetic flow liquid in the plastic bottles of capping and cover tightening seal;
Step 7, the plastic bottle that fills magnetic flow liquid that step 6 is obtained place the magnetic field of adjustable magnetic fields size, and magnetic field intensity is adjusted to 25mT;
Step 8, magnetic flow liquid was taken out from magnetic field in per 10 days, stir 5 minutes with glass bar after, 7 operations set by step again;
Step 9, after 25 days magnetic flow liquid is taken out from magnetic field, magnetic flow liquid has flowability, and no layering and agglomeration are stirred to uniform state with glass bar and promptly obtain stable silicone oil based magnetic rheologic liquid.
Claims (4)
1, a kind of silicone oil based magnetic rheologic liquid is characterized in that being become by following components in mass portion array:
65～90 parts of magnetic particles, 10～35 parts of the composite carrier fluids of silicone oil base of silicone oil doping preparation;
Wherein said magnetic particle is chelate surfactant/carbonyl iron core-shell type magnetic compound particle, and its particle diameter is 1～100 micron;
Described additive comprises following component by magnetic flow liquid gross mass percentage:
Thixotropic agent: 0.05%～2%, composition is nanometer lithium magnesium silicate, polysaccharide, cellulose derivative or bentonite;
Antioxidant: 0.1%～1%, composition is natrium nitrosum, Sodium Benzoate or monoethanolamine phosphate;
Antiwear additive: 1%～3%, composition is graphite, nano alumina powder or nano-cerium oxide powder;
Surfactant: 0.1%～3%, composition is N-lauroyl ethylenediamine triacetic acid, neopelex, oleic acid or polyether-based benzene sulfonic acid sodium salt.
2, the preparation method of the composite carrier fluid of claim 1 described magnetic flow liquid silicone oil base is characterized in that preparation process is:
Step 1, the amount of surfactant by magnetic flow liquid gross mass 0.1%～3% joined in the silicone oil, at room temperature mixed 3～5 hours, obtain suspension;
Step 2, antioxidant is joined in the suspension that step 1 obtains by the amount of magnetic flow liquid gross mass 0.1%～1%, at room temperature mixed 2～4 hours, obtain suspension;
Step 3, thixotropic agent is joined in the suspension that step 2 obtains by the amount of magnetic flow liquid gross mass 0.05%～2%, at room temperature mixed 2～4 hours, obtain suspension;
Step 4, antiwear additive is joined in the suspension that step 3 obtains by the amount of magnetic flow liquid gross mass 1%～3%, at room temperature mixed 2～4 hours, promptly make the composite carrier fluid of magnetic flow liquid silicone oil base.
3, the preparation method of the described magnetic flow liquid of claim 1 is characterized in that preparation process is:
Step 1, chelate surfactant/carbonyl iron core-shell type magnetic compound particle is joined in the composite carrier fluid of silicone oil base, stirs;
Step 2, the mixed material that step 1 is stirred join in the ball grinder, press 1: 10 mass ratio of mixed material and steel ball and add steel ball, with air in the nitrogen replacement jar, speed with 200～300 rev/mins, ball milling 3～10 hours, isolate steel ball, obtain magnetic flow liquid, sealing is protected and is preserved in the plastic bottles of the capping of packing into.
4, the post-processing approach of the described silicone oil based magnetic rheologic liquid of claim 1, it is characterized in that, to contain in plastic bottle by the silicone oil magnetic flow liquid that claim 3 newly makes and seal, place the magnetic field of adjustable magnetic fields size, magnetic field intensity is adjusted to 100～400mT, magnetic flow liquid was taken out from magnetic field in per 10 days, stir after 5～20 minutes, contain in plastic bottle and seal, place the magnetic field of adjustable magnetic fields size, magnetic field intensity is adjusted to 100～400mT, repeat aforesaid operations, after 20～60 days magnetic flow liquid is taken out from magnetic field, obtain stable silicone oil based magnetic rheologic liquid, sealing gets final product long preservation in the dry plastic bottle of packing into.
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