Summary of the invention
The object of the invention is to be to provide a kind of carbonyl iron dust that can strengthen magnetic rheology effect, and then provide magnetic flow liquid of a kind of efficient stable and preparation method thereof, this carbonyl iron dust is usingd diprotic acid as additive, has effectively improved yielding stress and the sedimentation stability of magnetic flow liquid.
Technical scheme of the present invention:
One of object of the present invention is to provide a kind of magnetic flow liquid carbonyl iron dust, and described carbonyl iron dust is to adopt diprotic acid carry out surface treatment according to the following steps and obtain:
Step 1, carbonyl iron dust is dry, removes surperficial planar water, and described carbonyl iron dust median size is 1-5 μ m, distribution spherical in shape, and purity is 99.9%;
Step 2, diprotic acid is joined in Virahol by 0.2%~2.5% of carbonyl iron dust quality, stir, obtain mixed solution after dissolved dilution, described diprotic acid is one or more combination of dimeracid, linoleic acid dimer, dodecanedioic acid;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed, and obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then add zirconium oxide balls, the mass ratio of mixture and abrading-ball is 1:(3~5), after milled, ball liquid is separated;
Step 5, that the suspension obtaining in step 4 is placed in to vacuum drying oven is dry, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
When the above magnetic flow liquid of preparation is used carbonyl iron dust, the vacuum tightness of the dry carbonyl iron dust of step 1 is-0.1~0.2MPa, and temperature is 70~100 ℃, time 12~16h.In step 5 step 5, dry vacuum tightness is-0.1~0.2MPa, 60~80 ℃ of temperature, time 6~9h.In step 3, ultrasonic wave jitter time is 15~30min.In step 4, adding zirconic diameter is 5~15mm, is preferably 10mm, and rotational speed of ball-mill 250~600rpm, is preferably 300rpm, time 6~8h.
Two of the object of the invention is to provide the magnetic flow liquid that adopts above carbonyl iron dust to prepare, and it consists of by mass percentage following component:
Surface treated carbonyl iron dust: 55%~89%
Base oil: 10%~42%
Thixotropic agent: 0.5%~1.5%
Slip additive: 0.5%~1.5%
Described base oil is methyl-silicone oil, mineral oil;
Described thixotropic agent is nano silicon, kaolin powder or organic clay;
Described slip additive is graphite, molybdenumdisulphide, boron nitride, tetrafluoroethylene, stearic acid, the combination of one or more in lauric acid or oleic acid.
Preparation process is:
Step 1, thixotropic agent is added in base oil by 0.5%~1.5% of magnetic flow liquid total mass, after stirring, ultrasonic wave is disperseed, and obtains mixed solution;
Step 2, slip additive is joined in the mixed solution that step 1 obtains by 0.5%~1.0% of magnetic flow liquid total mass, after stirring, ultrasonic wave is disperseed, and obtains mixed solution;
Step 3, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed, and obtains suspension;
Step 4, the suspension obtaining in step 3 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, after milled, ball liquid is separated, obtains magnetic flow liquid, packs sealing in dry plastic containers into and gets final product prolonged preservation.
In the preparation of above magnetic flow liquid, the ultrasonic wave jitter time 15~30min of step 1-step 3.The abrading-ball rotating speed of step 4 is 250~600rpm, is preferably 300rpm, and time 10~16h, is preferably 12h.
The invention provides a kind of new method and strengthen magnetic rheology effect, by using diprotic acid as additive, significantly improved the yielding stress of magnetic flow liquid.In addition, as a kind of effective dispersion agent, the composite use of diprotic acid and thixotropic agent, is conducive to improve the sedimentation stability of magnetic flow liquid,
Magnetic flow liquid of the present invention has sedimentation stability, friction and wear behavior and the chemical stability of significant magnetic rheology effect, excellence, and the feature such as low null field viscosity, and preparation technology is simple, cost is lower, can be widely used in the fields such as machinery, automobile, aviation, precision sizing, building, medical treatment.
Embodiment
In order to understand better the present invention, below in conjunction with example, further set forth content of the present invention, but content of the present invention is not only confined to the following examples.
The present invention adopts the senior rheometer of the MCR301 modularization intelligent type of Austrian Anton Paar company to measure the rheological characteristics of magnetic flow liquid.
The present invention adds 20ml magnetic flow liquid in graduated test tube, standing for a long time, observes the settling property that throw out characterizes magnetic flow liquid over time.
The carbonyl iron dust median size adopting in following example is 1-5 μ m, distribution spherical in shape, and purity is 99.9%.
Embodiment 1
Prepare 100 milliliters of (118.3 grams) silicone oil based magnetic rheologic liquids, preparation process is:
Step 1, by 78.4g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,1.2g dimeracid is joined in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6,0.8g nano silicon is joined in 42.5ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 7, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 6 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 8, the suspension obtaining in step 7 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.
Embodiment 2
Prepare 100 milliliters of (118.3g) silicone oil based magnetic rheologic liquids, preparation process is:
Step 1, by 78.4g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,1.2g dodecanedioic acid is joined in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6,0.8g nano silicon is added in 42.5ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 7, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 6 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 8, the suspension obtaining in step 7 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.
Embodiment 3
Prepare 100 milliliters of (117.5g) silicone oil based magnetic rheologic liquids, preparation process is:
Step 1, by 78.4g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,1.2g dimeracid is entered in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6, the carbonyl iron dust after surface treatment is joined in 42.5ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 7, the suspension obtaining in step 6 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.
Embodiment 4
Preparation 102.3g silicone oil based magnetic rheologic liquid, preparation process is:
Step 1, by 65g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,1.0g linoleic acid dimer is joined in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6,0.6g kaolin powder is joined in 40ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 7, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 6 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 8, the suspension obtaining in step 7 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.
Embodiment 5
Preparation 103.7g silicone oil based magnetic rheologic liquid, preparation process is:
Step 1, by 65g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,0.8g linoleic acid dimer is joined in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6,1.0g polyorganosilicate is joined in 40ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 7,1.2g tetrafluoroethylene is joined in the mixed solution that step 6 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 8, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 7 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 9, the suspension obtaining in step 8 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.
Embodiment 6
Preparation 112.9g silicone oil based magnetic rheologic liquid, preparation process is:
Step 1, by 70g carbonyl iron dust, in vacuum tightness, be that 0.1MPa, temperature are dry 12h under 70 ℃ of conditions, remove surperficial physical absorption water;
Step 2,1.0g dodecanedioic acid is joined in 35ml Virahol, stir, after dissolved dilution, obtain mixed solution;
Step 3, dry carbonyl iron dust is joined in the mixed solution that step 2 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 4, the suspension obtaining in step 3 is packed in ball grinder, then to add diameter be the zirconium oxide balls of 10mm, the mass ratio of mixture and abrading-ball is 1:3, with rotating speed ball milling 6~8h of 300rpm, after milled, ball liquid is separated;
Step 5, the suspension obtaining in step 4 being placed in to electric vacunm drying case, is that 0.1MPa, temperature are dry 6h under 70 ℃ of conditions in vacuum tightness, the blocks of solid of gained is pulverized after dry and obtains the carbonyl iron dust after surface treatment.
Step 6,0.75g kaolin powder is joined in 45ml methyl-silicone oil, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 7,1.0g graphite is joined in the mixed solution that step 6 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains mixed solution;
Step 8, the carbonyl iron dust after surface treatment is joined in the mixed solution that step 7 obtains, after stirring, ultrasonic wave is disperseed 20min, obtains suspension;
Step 9, the suspension obtaining in step 8 being placed in to ball grinder, is that 1:3 adds zirconium oxide balls by the mass ratio of mixture and abrading-ball, with the rotating speed ball milling 12h of 300rpm, after milled, ball liquid is separated, obtains magnetic flow liquid.