CN108364743B - Three-phase magnetorheological fluid and preparation method thereof - Google Patents
Three-phase magnetorheological fluid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a three-phase magnetorheological fluid and a preparation method thereof, wherein the three-phase magnetorheological fluid comprises the following components in percentage by volume: magnetic particles: 5-40%, carrier liquid: 60-90%, magnetic fluid: 0.5-15%, emulsifier: 0.05-5% of cosurfactant and 0.03-3% of cosurfactant. The magnetic material has the advantages of low zero field viscosity, high magnetic energy storage modulus, strong magneto-rheological effect, simple preparation method and low cost.
Description
Technical Field
The invention relates to the technical field of intelligent materials and preparation, in particular to a three-phase magnetorheological fluid and a preparation method thereof.
Background
The magnetorheological fluid is a two-phase suspension system formed by uniformly dispersing micron-scale magnetic solid particles in a liquid medium, and the physical state and rheological property of the magnetorheological fluid can change along with the change of an external magnetic field: under the action of no external magnetic field, the fluid shows a good flowing state, and under the action of strong magnetic field, the viscosity can be instantly increased by more than two orders of magnitude, and the fluid shows the mechanical property similar to solid, and becomes free flowing fluid once the magnetic field is removed.
The prepared magnetorheological material with high magnetocaloric effect and relative stability has attractive application value. In general, the yield stress of a magnetorheological fluid can be increased by increasing the content of magnetic particles or the current intensity. But will lead to the zero field viscosity of the magnetic rheological liquid to be increased, the mass and the size of the magnetic rheological device to be increased, and simultaneously, the electric load of the magnetic rheological device can be increased. The choice of alloy particles or non-spherical particles with a greater saturation magnetization can enhance the magnetorheological effect, however for most practical applications the materials are complex to prepare and costly. The shear yield stress of the magnetorheological fluid can be increased by the squeeze mode or the electromagnetic field synergistic effect at the expense of increased equipment complexity. Therefore, the research on the theory and method for enhancing the magnetorheological effect is still one of the problems to be solved in the engineering application of the magnetorheological material.
Disclosure of Invention
The invention aims to provide a three-phase magnetorheological fluid and a preparation method thereof, wherein the three-phase magnetorheological fluid has low zero-field viscosity, high magnetic storage energy modulus, stronger magnetorheological effect, simple preparation method and low cost.
The three-phase magnetorheological fluid consists of the following components in percentage by volume:
magnetic particles: 5-40%, carrier liquid: 60-90%, magnetic fluid: 0.5-15%, emulsifier: 0.05-5% of cosurfactant and 0.03-3% of cosurfactant.
Furthermore, the magnetic particles are carbonyl iron powder or magnetic ferrite powder, and the average particle size of the magnetic particles is 1-10 mu m.
Further, the carrier liquid is a combination of one or more of water, alcohol, alkane, vegetable oil, mineral oil, silicone oil, and polyalphaolefin.
Further, the magnetic fluid is a water-based magnetic fluid or an oil-based magnetic fluid and comprises a solvent and magnetic particles with the particle size of 3-15 nm ultrasonically dispersed in the solvent, wherein the magnetic particles are gamma-Fe2O3、Fe3O4Or iron-cobalt-nickel alloy nano particles, the volume percentage of which in the magnetic fluid is 0.1-2%; when the magnetic fluid is water-based magnetic fluid and the carrier fluid is oil-based, the emulsifier is one or a combination of more of divalent metal soap salt, lanolin, cholesterol, polyether and polyester; when the magnetic fluid is oil-based and the carrier liquid is water-based, the emulsifier is one or more of monovalent metal soap salt, polyester, polyvinyl alcohol, sodium carboxymethyl cellulose, polyether, lecithin, Arabic gum, gelatin and seaweed gel.
Further, the cosurfactant is a small molecular acid, alcohol or ketone.
A preparation method of a three-phase magnetorheological fluid comprises the following steps:
1) taking a proper amount of magnetic particles and drying;
2) dissolving an emulsifier and a cosurfactant into carrier liquid, adding magnetic fluid, stirring for 2-20 min under the condition that the rotating speed is 800-3000 rmp, and then performing ultrasonic emulsification for 2-10 min to obtain magnetic microemulsion;
3) adding the magnetic particles dried in the step 1) into the magnetic microemulsion obtained in the step 2), stirring for 2-20 min under the condition that the rotating speed is 800-3000 rmp, and then dispersing for 1-5 min by ultrasonic waves; the high-speed stirring is to carry out coarse dispersion on the magnetic fluid, so that the magnetic fluid is prevented from volatilizing due to temperature rise during ultrasonic dispersion;
4) and (3) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove air bubbles to obtain the three-phase magnetorheological fluid, and placing the three-phase magnetorheological fluid in a dry plastic container to seal the container so as to be preserved for a long time.
Further, the vacuum degree of the dried magnetic particles in the step 1) is 0.2MPa, the temperature is 80-100 ℃, and the time is 6-12 h.
Further, the vacuum degree in the vacuum drying oven in the step 4) is 0.2-0.6 MPa, and bubbles are removed for 5-30 min at normal temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the three-phase magnetorheological fluid consists of magnetic particles, magnetic fluid and carrier fluid, wherein the magnetic fluid is used as a magnetic repairing material to fill gaps in a chain structure of the magnetic particles, so that the magnetic conductivity of the particle chain is improved, the interaction among the magnetic particles is increased, and the mechanical property of the magnetorheological material is improved.
2. The invention prepares stable magnetic current micro-emulsion by selecting specific emulsifier and cosurfactant, and then adds magnetic fluid into the magnetic current liquid in a stable liquid drop form as a third phase to enhance the magnetic current change effect.
Drawings
FIG. 1 is a graph of storage modulus versus magnetic field strength for a three-phase magnetorheological fluid of an example two of the present invention and a comparative example one;
FIG. 2 is a graph of storage modulus versus magnetic field strength for a three-phase magnetorheological fluid of example three and a comparative example two in accordance with the present invention;
FIG. 3 is a graph of storage modulus versus magnetic field strength for a three-phase magnetorheological fluid according to a fourth example of the invention and a comparative example three;
fig. 4 is a graph of the storage modulus versus magnetic field strength for a three-phase magnetorheological fluid according to example five of the present invention and a comparative sample four.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
In one embodiment, a three-phase magnetorheological fluid is characterized in that: the composition comprises the following components in percentage by volume:
magnetic particles: 5-40%, carrier liquid: 60-90%, magnetic fluid: and (3) an emulsifier: 0.05-5% of cosurfactant and 0.03-3% of cosurfactant;
the magnetic particles are carbonyl iron powder or magnetic ferrite powder, and the average particle size of the magnetic particles is 1-10 mu m.
The carrier liquid is one or more of water, alcohol, alkane, vegetable oil, mineral oil, silicone oil and poly alpha olefin;
the magnetic fluid is a water-based magnetic fluid or an oil-based magnetic fluid and comprises a solvent and magnetic particles with the particle size of 3-15 nm ultrasonically dispersed in the solvent, wherein the magnetic particles are gamma-Fe2O3、Fe3O4Or Fe-Co-Ni alloy nanoparticles, the volume percentage of which in the magnetic fluid is 0.1-2%.
When the magnetic fluid is water-based magnetic fluid and the carrier fluid is oil-based, the emulsifier is one or a combination of more of divalent metal soap salt, lanolin, cholesterol, polyether and polyester; when the magnetic fluid is oil-based and the carrier liquid is water-based, the emulsifier is one or more of lecithin such as monovalent metal soap salt, polyester, polyvinyl alcohol, sodium carboxymethyl cellulose, polyether and the like, acacia, gelatin and seaweed gel.
The cosurfactant is a small molecular acid, alcohol or ketone.
In a second embodiment, a method for preparing a three-phase magnetorheological fluid comprises the following steps:
1) taking 0.78g of carbonyl iron powder, drying for 15h under the conditions that the vacuum degree is 0.1MPa and the temperature is 90 ℃, and removing the physical adsorption water on the surface of the carbonyl iron powder;
2) preparing magnetic fluid, and preparing Fe by chemical coprecipitation method3O4Magnetic particles, which are specifically prepared by the following steps;
a. mixing ferrous salt and ferric salt according to a certain proportion, adding precipitator ammonia water solution, stirring, reacting for a period of time to obtain black Fe3O4Colloidal particle precipitation, the reaction formula is:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O；
b. washing black precipitate with water, separating, adding HNO3The solution is stirred and then Fe (NO) is added3)3Boiling the solution for a period of time to obtain gamma-Fe2O3A brown precipitate;
c. dispersing the brown precipitate in a sodium citrate aqueous solution, adjusting the temperature to 80 ℃ and the pH =7, and performing surface treatment;
d, dispersing the precipitate treated in the step c in deionized water after solvent washing and citric acid treatment, adjusting the pH =7, and centrifuging for 1h to separate larger particles and aggregates to prepare the magnetic fluid, wherein Fe in the magnetic fluid3O4The volume fraction of the magnetic particles is 1%, and the magnetic fluid obtained by test verification has no sedimentation and phase separation phenomenon within months;
3) emulsifiers Tween60 and Span80 were mixed at 1: dissolving the 9 into 9.95 ml of mineral oil, adding 0.2ml of ethanol with the purity of 99.9%, uniformly stirring, adding 0.05 ml of magnetofluid, stirring for 3min under the condition that the rotating speed is 1500rmp, and performing ultrasonic emulsification for 5min to obtain magnetic microemulsion, wherein the particle size of emulsion droplets is about 150-250 nm;
3) adding the magnetic particles dried in the step 1) into 1.9ml of magnetic microemulsion obtained in the step 2), stirring for 5min under the condition that the rotating speed is 1000rmp, and then dispersing for 2min by ultrasonic waves;
4) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove bubbles, wherein the vacuum degree is 0.2MPa, and removing the bubbles for 10min at normal temperature to obtain the three-phase magnetorheological fluid, wherein the three-phase magnetorheological fluid comprises the following components: carbonyl iron powder 5vol%, mineral oil 91.125vol%, magnetic fluid 0.475vol%, emulsifier 1.9vol%, and co-surfactant 1.5 vol%.
In a third embodiment, a method for preparing a three-phase magnetorheological fluid comprises the following steps:
1) 1.56g of carbonyl iron powder is dried for 15 hours under the conditions that the vacuum degree is 0.1MPa and the temperature is 90 ℃, and the physical adsorption water on the surface of the carbonyl iron powder is removed;
2) preparing magnetic fluid, and preparing Fe by chemical coprecipitation method3O4Magnetic particles, which are specifically prepared by the following steps;
a. mixing ferrous salt and ferric salt according to a certain proportion, adding precipitator ammonia water solution, stirring, reacting for a period of time to obtain black Fe3O4Colloidal particle precipitation, the reaction formula is:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O；
b. washing black precipitate with water, separating, adding HNO3The solution is stirred and then Fe (NO) is added3)3Boiling the solution for a period of time to obtain gamma-Fe2O3A brown precipitate;
c. dispersing the brown precipitate in a sodium citrate aqueous solution, adjusting the temperature to 80 ℃ and the pH =7, and performing surface treatment;
d, dispersing the precipitate treated in the step c in deionized water after solvent washing and citric acid treatment, adjusting the pH =7, and centrifuging for 1h to separate larger particles and aggregates to prepare the magnetic fluid, wherein Fe in the magnetic fluid3O4The volume fraction of the magnetic particles is 1%, and the magnetic fluid obtained by test verification has no sedimentation and phase separation phenomenon within months;
3) emulsifiers Tween60 and Span80 were mixed at 1: dissolving the 9 into 9.9 ml of mineral oil, adding 0.195ml of ethanol with the purity of 99.9%, uniformly stirring, adding 0.1ml of magnetofluid, stirring for 5min under the condition that the rotating speed is 1500rmp, and performing ultrasonic emulsification for 5min to obtain magnetic microemulsion, wherein the particle size of emulsion droplets is about 150-250 nm;
3) adding the magnetic particles dried in the step 1) into 1.8ml of the magnetic microemulsion obtained in the step 2), stirring for 5min under the condition that the rotating speed is 1000rmp, and then dispersing for 2min by ultrasonic waves;
4) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove bubbles, wherein the vacuum degree is 0.2MPa, and removing the bubbles for 10min at normal temperature to obtain the three-phase magnetorheological fluid, wherein the three-phase magnetorheological fluid comprises the following components: 10vol% of carbonyl iron powder, 85.7vol% of mineral oil, 0.9vol% of magnetic fluid, 1.8vol% of emulsifier and 1.6vol% of cosurfactant.
In a fourth embodiment, a method for preparing a three-phase magnetorheological fluid comprises the following steps:
1) 2.34g of carbonyl iron powder is taken and dried for 15 hours under the conditions that the vacuum degree is 0.1MPa and the temperature is 90 ℃, and the physical adsorption water on the surface of the carbonyl iron powder is removed;
2) preparing magnetic fluid, and preparing Fe by chemical coprecipitation method3O4Magnetic particles, which are specifically prepared by the following steps;
a. mixing ferrous salt and ferric salt according to a certain proportion, adding precipitator ammonia water solution, stirring, reacting for a period of time to obtain black Fe3O4Colloidal particle precipitation, the reaction formula is:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O；
b. washing black precipitate with water, separating, adding HNO3The solution is stirred and then Fe (NO) is added3)3Boiling the solution for a period of time to obtain gamma-Fe2O3A brown precipitate;
c. dispersing the brown precipitate in a sodium citrate aqueous solution, adjusting the temperature to 80 ℃ and the pH =7, and performing surface treatment;
d, washing the precipitate treated in the step c by using a solvent and treating the precipitate by using citric acidDispersing the mixture in deionized water after treatment, adjusting the pH =7, centrifuging for 1h to separate larger particles and aggregates to prepare the magnetic fluid, wherein Fe in the magnetic fluid3O4The volume fraction of the magnetic particles is 1%, and the magnetic fluid obtained by test verification has no sedimentation and phase separation phenomenon within months;
3) emulsifiers Tween60 and Span80 were mixed at 1: dissolving the 9 into 9.5 ml of mineral oil, adding 0.175ml of ethanol with the purity of 99.9%, uniformly stirring, adding 0.5 ml of magnetofluid, stirring for 5min under the condition that the rotating speed is 1800rmp, and performing ultrasonic emulsification for 5min to obtain a magnetic microemulsion, wherein the particle size of emulsion droplets is about 150-250 nm;
3) adding the magnetic particles dried in the step 1) into 1.7ml of magnetic microemulsion obtained in the step 2), stirring for 5min under the condition that the rotating speed is 1000rmp, and then dispersing for 3min by ultrasonic waves;
4) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove bubbles, wherein the vacuum degree is 0.2MPa, and removing the bubbles for 10min at normal temperature to obtain the three-phase magnetorheological fluid, wherein the three-phase magnetorheological fluid comprises the following components: carbonyl iron powder 15vol%, mineral oil 77.55vol%, magnetic fluid 4.25vol%, emulsifier 1.7vol%, and co-surfactant 1.5 vol%.
In a fifth embodiment, a method for preparing a three-phase magnetorheological fluid comprises the following steps:
1) 2.34g of carbonyl iron powder is taken and dried for 15 hours under the conditions that the vacuum degree is 0.1MPa and the temperature is 90 ℃, and the physical adsorption water on the surface of the carbonyl iron powder is removed;
2) preparing magnetic fluid, and preparing Fe by chemical coprecipitation method3O4Magnetic particles, which are specifically prepared by the following steps;
a. mixing ferrous salt and ferric salt according to a certain proportion, adding precipitator ammonia water solution, stirring, reacting for a period of time to obtain black Fe3O4Colloidal particle precipitation, the reaction formula is:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O；
b. washing the black precipitate with waterAfter separation, HNO is added3The solution is stirred and then Fe (NO) is added3)3Boiling the solution for a period of time to obtain gamma-Fe2O3A brown precipitate;
c. dispersing the brown precipitate in a sodium citrate aqueous solution, adjusting the temperature to 80 ℃ and the pH =7, and performing surface treatment;
d, dispersing the precipitate treated in the step c in deionized water after solvent washing and citric acid treatment, adjusting the pH =7, and centrifuging for 1h to separate larger particles and aggregates to prepare the magnetic fluid, wherein Fe in the magnetic fluid3O4The volume fraction of the magnetic particles is 1%, and the magnetic fluid obtained by test verification has no sedimentation and phase separation phenomenon within months;
3) emulsifiers Tween60 and Span80 were mixed at 1: dissolving the 9 into 9.2 ml of mineral oil, adding 0.17ml of ethanol with the purity of 99.9%, uniformly stirring, adding 0.8ml of magnetofluid, stirring for 5min under the condition that the rotating speed is 2000rmp, and performing ultrasonic emulsification for 5min to obtain a magnetic microemulsion, wherein the particle size of emulsion droplets is about 200-400 nm;
3) adding the magnetic particles dried in the step 1) into 1.7ml of the magnetic microemulsion obtained in the step 2), stirring for 5min under the condition that the rotating speed is 1500rmp, and then dispersing for 3min by ultrasonic waves;
4) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove bubbles, wherein the vacuum degree is 0.2MPa, and removing the bubbles for 10min at normal temperature to obtain the three-phase magnetorheological fluid, wherein the three-phase magnetorheological fluid comprises the following components: carbonyl iron powder vol%, mineral oil 75vol%, magnetic fluid 6.8vol%, emulsifier 1.7vol%, and co-surfactant 1.5 vol%.
Example six, the prepared three-phase magnetorheological fluid was subjected to comparative analysis:
taking the three-phase magnetorheological fluid prepared in the second embodiment as an analysis sample I, and taking the magnetorheological fluid with the carbonyl iron powder content of 5vol% as a comparison sample I;
taking the three-phase magnetorheological fluid prepared in the third embodiment as an analysis sample II, and taking the magnetorheological fluid with the carbonyl iron powder content of 10vol% as a comparison sample II;
taking the three-phase magnetorheological fluid prepared in the fourth embodiment as an analysis sample III, and taking the magnetorheological fluid with the carbonyl iron powder content of 15vol% as a comparison sample III;
taking the three-phase magnetorheological fluid prepared in the fifth embodiment as an analysis sample IV and taking the magnetorheological fluid with the carbonyl iron powder content of 15vol% as a comparison sample IV;
referring to fig. 1 to 4, the storage modulus of the first analysis sample, the second analysis sample, the third analysis sample and the fourth analysis sample is respectively higher than that of the first comparison sample, the second comparison sample, the third comparison sample and the fourth comparison sample, which shows that the three-phase magnetorheological fluid has better magnetorheological effect, and simultaneously, because the consumption of the magnetic fluid is less, the viscosity of the emulsified carrier is similar to the basic viscosity, the magnetorheological effect of the magnetorheological material can be obviously enhanced under the condition of not changing the zero-field viscosity of the magnetorheological fluid.
Claims (7)
1. A three-phase magnetorheological fluid is characterized in that: the composition comprises the following components in percentage by volume:
magnetic particles: 5-40%, carrier liquid: 60-90%, magnetic fluid: 0.5-15%, emulsifier: 0.05-5% of cosurfactant and 0.03-3% of cosurfactant;
the magnetic fluid is a water-based magnetic fluid and comprises a solvent and magnetic particles gamma-Fe with the particle size of 3-15 nm and ultrasonically dispersed in the solvent2O3、Fe3O4Or Fe-Co-Ni alloy nanoparticles, the magnetic particles being gamma-Fe2O3Or Fe3O4Or the volume percentage of the iron-cobalt-nickel alloy nano particles in the magnetic fluid is 0.1-2%;
when the magnetic fluid is water-based and the carrier fluid is oil-based, the emulsifier is one or a combination of more of divalent metal soap salt, lanolin, cholesterol, polyether and polyester.
2. The three-phase magnetorheological fluid of claim 1, wherein: the magnetic particles are carbonyl iron powder or magnetic ferrite powder, and the average particle size of the magnetic particles is 1-10 mu m.
3. The three-phase magnetorheological fluid according to claim 1 or 2, wherein: the carrier fluid is one of alcohol, vegetable oil, mineral oil, silicone oil and poly alpha olefin.
4. The three-phase magnetorheological fluid according to claim 1 or 2, wherein: the cosurfactant is a small molecular acid, alcohol or ketone.
5. A preparation method of the three-phase magnetorheological fluid according to any one of claims 1 to 4, characterized by comprising the following steps:
1) taking a proper amount of magnetic particles and drying;
2) dissolving an emulsifier and a cosurfactant into carrier liquid, adding magnetic fluid, stirring for 2-20 min under the condition that the rotating speed is 800-3000 rmp, and then performing ultrasonic emulsification for 2-10 min to obtain magnetic microemulsion;
3) adding the magnetic particles dried in the step 1) into the magnetic microemulsion obtained in the step 2), stirring for 2-20 min under the condition that the rotating speed is 800-3000 rmp, and then dispersing for 1-5 min by ultrasonic waves;
4) and (3) placing the magnetorheological fluid treated in the step 3) in a vacuum drying oven to remove air bubbles to obtain the three-phase magnetorheological fluid, and placing the three-phase magnetorheological fluid in a dry plastic container to seal the container so as to be preserved for a long time.
6. The method for preparing a three-phase magnetorheological fluid according to claim 5, wherein: the vacuum degree of the dried magnetic particles in the step 1) is 0.2MPa, the temperature is 80-100 ℃, and the time is 6-12 h.
7. The method for preparing a three-phase magnetorheological fluid according to claim 6, wherein: and 4) in the step 4), the vacuum degree in the vacuum drying oven is 0.2-0.6 MPa, and bubbles are removed for 5-30 min at normal temperature.
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| CN112552987A (en) * | 2021-01-19 | 2021-03-26 | 江西赛诺得新材料有限公司 | Preparation method of ultra-stable silicone oil-based magnetorheological fluid |
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