CN107043647B - A kind of giant electro-rheological liquid dielectric grain and preparation method thereof - Google Patents
A kind of giant electro-rheological liquid dielectric grain and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of giant electro-rheological liquid dielectric grains, are nanometer core-shell structure composite material, using doping type titanium dioxide as core, surface is coated with polar polymer；The doping type titanium dioxide is to adulterate high dielectric constant organic matter in titanium dioxide preparation process to be prepared；Wherein, titanium dioxide accounts for 80%~90%, and high dielectric constant organic matter accounts for 5%~10%, and polar polymer accounts for 5%~10%.Preparation method are as follows: (1) when preparing nano-titanium dioxide, high dielectric constant organic matter is added, prepares doping type titanium dioxide；(2), by the way that polar polymer is added in in-situ polymerization normal direction doping type titanium dioxide, giant electro-rheological liquid dielectric grain is obtained.The features such as dielectric grain of the invention, dielectric constant with higher, resistance to settling are good, particle size is nanoscale, is pollution-free；When being used for giant electro-rheological liquid, has many advantages, such as good electric rheological effect, high and low temperature resistance is good, long-term place does not settle.
Description
Technical field
The present invention relates to a kind of giant electro-rheological liquid dielectric grains and preparation method thereof, belong to new material technology field.
Background technique
Giant electro-rheological liquid (GRF) is a kind of colloid being uniformly suspended in non-conductive continuous phase by dielectric grain, when right
When GRF applies the electric field of some strength, change can be immediately occurred in rheological property, become class solid state from liquid, when cancelling electricity
When field, and recover immediately into original liquid.Giant electro-rheological liquid has the characteristics that following in the electric field: (1) in liquid and class
It being quickly converted between solid, i.e., apparent viscosity can great changes will take place under static or low shear rate, with solid properties
Anti-shear ability；(2) liquid it is solid between conversion be reversible；(3) liquid it is solid between conversion be it is controllable, only need to be to electric field signal
It is controlled；(4) change of apparent viscosity is the variation with electric field strength and consecutive variations；(5) liquid it is solid between conversion,
The change of apparent viscosity can be completed within millisecond, and response speed is high；(6) energy for controlling phase transformation is extremely low.These are excellent
Performance become a kind of very potential novel intelligent material, can be widely applied to mechanical engineering, automobile industry, aviation
The fields such as space flight, national defence.
Electric rheological effect originates from the polarization and interparticle interaction of dielectric grain under electric field action, so, electric current
The power for becoming fluidity energy is mainly determined by dielectric grain.Therefore, dielectric grain is the important composition of giant electro-rheological liquid.Dielectric grain
It can be inorganic matter (such as barium titanate, titanium dioxide), organic polymer (such as macromolecule polymer material, semiconducting polymer
Material) or compound material (such as organic matter coated inorganic object).When with inorganic matter as dielectric grain, dielectric constant is higher, but
The defects of there are density greatly, particle suspension stability is poor, quality is harder, the abrasion for becoming device to electric current is larger, and shear strength is still
It needs to further increase.When with organic polymer as dielectric grain, very high shear strength can achieve, but it exists in height
The disadvantages of leakage current density is larger under voltage, height temperature stability is poor, environmental pollution is more serious.Compound material is more typical
It is nucleocapsid structure, feature are as follows: the dielectric constant of particle can be improved in highly conductive core, adds the surface charge of particle, and mentions
For conductivity appropriate；The resistance to electric field breakdown ability of material and effectively limitation table can be improved in the insulating outer layer of high dielectric constant
The movement of surface charge, at the same improve chain structure stability and electric rheological effect it is stronger (shear strength is bigger).
Summary of the invention
For the above-mentioned prior art, a kind of giant electro-rheological liquid dielectric grain and preparation method thereof
The present invention provides one kind can enable giant electro-rheological liquid is stable, resistance to settling is good, shear strength is big, to device without corruption
Erosion, free of contamination giant electro-rheological liquid dielectric grain；The present invention also provides preparation methods.
The present invention is achieved by the following technical solutions:
A kind of giant electro-rheological liquid dielectric grain is nanometer core-shell structure composite material, is with doping type titanium dioxide
Core, surface are coated with polar polymer；The doping type titanium dioxide is that high dielectric is adulterated in titanium dioxide preparation process is normal
Number organic matter is prepared；Wherein, the mass fraction of titanium dioxide is 80%~90%, the quality of high dielectric constant organic matter
Score is 5%~10%, and the mass fraction of polar polymer is 5%~10%.
The high dielectric constant organic matter is in Kynoar (PVDF), polyvinyl fluoride (PVF), polyimides (PI)
It is one or more.
The polar polymer is in polyacrylonitrile, polyethylene terephthalate, polyvinyl alcohol, polyaniline (PAN)
It is one or more.
Giant electro-rheological liquid dielectric grain of the invention is in the cladding polar polymer preparation of doping type titanium dioxide surface
Made of；The doping type titanium dioxide is to adulterate high dielectric constant organic matter in titanium dioxide preparation process to be prepared
's.
The preparation method of the giant electro-rheological liquid dielectric grain, comprising the following steps:
(1) 60~120mL titanate is dissolved in 60~120mL dehydrated alcohol and (stirs 30~60min at room temperature), be denoted as
A liquid；
The titanate is in isopropyl titanate, tetraisopropyl titanate, butyl titanate, positive four butyl ester of metatitanic acid, barium titanate
It is one or more；
(2) 0.6~1.6g high dielectric constant organic matter is dissolved in 10~20mL dehydrated alcohol and (descends uniform stirring at room temperature
15~30min), it is denoted as B liquid；
(3) B liquid is added dropwise in A liquid, (control reaction process is not in 0.17~0.35mL/min for control rate of titration
Less than 1h)；Reaction is to white precipitate is no longer generated, by the white precipitate washes of absolute alcohol of generation, to remove white precipitate
In impurity；
(4) white precipitate after above-mentioned cleaning is dried in vacuo 2~5h at 60~80 DEG C to get doping type titanium dioxide；
(5) 0.6~1.6g polar polymer is dissolved in 10~20mL dehydrated alcohol to (heating water bath is stirred to 30~60 DEG C
Mix to being completely dissolved, and be cooled to room temperature), obtain polar polymer solution；
(6) it by the doping type titanium dioxide of step (4), is added in the polar polymer solution of step (5), adjusts pH value
(being adjusted with concentrated hydrochloric acid or hydrochloric acid) is 4.0~5.5, and ultrasonic disperse stirs 10~20min, keeps doping type titanium dioxide fully dispersed
In polar polymer solution, white suspension is formed；
(7) above-mentioned white suspension is heated to 45~60 DEG C, reacts 20~40min；After reaction, it is cooled to room
Temperature, adjusting pH value with alkaline solution is 6.8~7.2；
The alkaline solution is in sodium hydroxide solution, potassium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution
It is one or more；
(8) solution of step (7) is filtered, gained solid matter is dried in vacuo 2~4h, powder at 40~50 DEG C after filtering
It is broken to get giant electro-rheological liquid dielectric grain.
Giant electro-rheological liquid dielectric grain of the invention, can be used for giant electro-rheological liquid, compared with prior art, have as follows
Advantage:
(1) in existing dielectric grain preparation process, only using single metal oxide as core；The present invention is preparing dielectric grain
Core when, adulterate a small amount of high dielectric constant polymer, the dielectric constant of dielectric grain on the one hand can be improved, on the other hand mix
Miscellaneous high dielectric constant polymer can be reacted with the polar polymer of clad, improve the stability of clad.
(2) dielectric grain in the prior art, density is uncontrollable in preparation process；The present invention when preparing dielectric grain,
The amount of clad is controlled by the reaction time, and then controls the density and the continuous phase density phase of giant electro-rheological liquid of dielectric grain
Closely, the resistance to settling energy of giant electro-rheological liquid is greatly improved.
When dielectric grain of the invention is used for giant electro-rheological liquid, have preferable electric rheological effect, shear strength high, anti-heavy
The advantages that performance is good, corrosion-free to device, pollution-free drops.Preparation method of the invention, simple process, securely and reliably, operation side
Just, economic and environment-friendly, it is easy to large-scale production.
Detailed description of the invention
Fig. 1: the structure schematic diagram of giant electro-rheological liquid dielectric grain of the invention, wherein 1, which represents high dielectric constant, has
Machine object, 2 represent nano-titanium dioxide, and 3 represent polar polymer.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Instrument involved in following embodiments, reagent, material etc. are unless otherwise noted existing in the prior art
Conventional instrument, reagent, material etc., can be obtained by regular commercial sources.Experimental method involved in following embodiments, inspection
Survey method etc. is unless otherwise noted existing routine experiment method in the prior art, detection method etc..
Embodiment 1
Steps are as follows:
(1) 60mL isopropyl titanate is dissolved in 60mL dehydrated alcohol, stirs 30min at room temperature, obtained uniform solution and be denoted as
A liquid.
(2) 1.0g polyvinyl fluoride is dissolved in 15mL dehydrated alcohol, stirs 20min at room temperature, obtained uniform solution and be denoted as B
Liquid.
(3) B liquid is added dropwise in A liquid, the rate of titration 0.25mL/min for controlling solution (it is not small to control reaction process
In 1h)；Reaction is to white precipitate is no longer generated, with washes of absolute alcohol, to remove the impurity in white precipitate.
(4) the white precipitate by step (3) is dried in vacuo 2h at 80 DEG C, obtains required polyimides doping titanium dioxide
Titanium.
(5) 1.5g polyaniline is dissolved in 15mL dehydrated alcohol, heating water bath is warming up to 55 DEG C, and stirring is and cold to being completely dissolved
But room temperature is arrived.
(6) the polyvinyl fluoride of step (4) is titania-doped, it is molten to be added to the polyaniline for having cooled to room temperature of step (5)
In liquid, adjusting pH value with concentrated hydrochloric acid is 4.5, and ultrasonic disperse stirs 18min, makes the titania-doped fully dispersed shape of polyimides
At white suspension.
(7) the white suspension of step (6) is heated to 50 DEG C, reacts 20min.After reaction, it is cooled to room temperature, uses hydrogen
It is 7.1 that sodium hydroxide solution, which is neutralized to pH value,.
(8) the solution of step (7) is filtered, in 50 DEG C of vacuum drying 2h, to get giant electro-rheological liquid polyvinyl alcohol after crushing
The titania-doped dielectric grain of polyimides is coated, structure diagram is as shown in Figure 1.
(9) by polyvinyl alcohol cladding, polyimides is titania-doped is dispersed in amido silicon oil, polyvinyl alcohol cladding
The titania-doped concentration of polyimides is 5g/mL, as giant electro-rheological liquid；Through detecting, the shearing of the giant electro-rheological liquid is strong
It spends 40.7KPa (voltage 3kV), dynamic viscosity 90.9Pas (voltage 3kV, shear rate 100s-1), response time 3ms, room temperature is close
Envelope is placed 30 days and is not settled.
Embodiment 2
Steps are as follows:
(1) 100mL butyl titanate is dissolved in 100mL dehydrated alcohol, stirs 50min at room temperature, obtained uniform solution and be denoted as
A liquid.
(2) 1.6g Kynoar is dissolved in 20mL dehydrated alcohol, stirs 30min at room temperature, obtained uniform solution and be denoted as
B liquid.
(3) B liquid is added dropwise in A liquid, the rate of titration 0.35mL/min for controlling solution (it is not small to control reaction process
In 1h)；Reaction is to white precipitate is no longer generated, with washes of absolute alcohol, to remove the impurity in white precipitate.
(4) the white precipitate by step (3) is dried in vacuo 3h at 70 DEG C, and as Kynoar is titania-doped.
(5) 1.3g polyacrylonitrile is dissolved in 15mL dehydrated alcohol, heating water bath is warming up to 50 DEG C, stirring to being completely dissolved, and
It is cooled to room temperature.
(6) the Kynoar of step (4) is titania-doped, it is added to the polypropylene for having cooled to room temperature of step (5)
In nitrile solution, adjusting pH value with concentrated hydrochloric acid is 5.0, and ultrasonic disperse stirs 15min, keeps Kynoar titania-doped sufficiently
Dispersion forms white suspension.
(7) the white suspension of step (6) is heated to 60 DEG C, reacts 40min.After reaction, it is cooled to room temperature, uses carbon
It is 7.0 that sour hydrogen sodium solution, which is neutralized to pH value,.
(8) step solution (7) is filtered, 3.5h is dried in vacuo at 45 DEG C, to get giant electro-rheological liquid with poly- third after crushing
Alkene nitrile coats the titania-doped dielectric grain of Kynoar.
(9) by polyacrylonitrile cladding, Kynoar is titania-doped is dispersed in amido silicon oil, polyacrylonitrile packet
Covering the titania-doped concentration of Kynoar is 2g/mL, as giant electro-rheological liquid；Through detecting, which is cut
Shearing stress 38.8KPa (voltage 3kV), dynamic viscosity 89.6Pas (voltage 3kV, shear rate 100s-1), response time 3ms, often
Temperature sealing, which is placed 30 days, not to be settled.
Embodiment 3
Steps are as follows:
(1) positive four ester of 120mL metatitanic acid is dissolved in 120mL dehydrated alcohol, stirs 60min at room temperature, obtain uniform solution note
For A liquid.
(2) 0.8g polyimides is dissolved in 12mL dehydrated alcohol, stirs 18min at room temperature, obtained uniform solution and be denoted as B
Liquid.
(3) B liquid is added dropwise in A liquid, the rate of titration 0.18mL/min for controlling solution (it is not small to control reaction process
In 1h)；Reaction is to white precipitate is no longer generated, with washes of absolute alcohol, to remove the impurity in white precipitate.
(4) the white precipitate by step (3) is dried in vacuo 5h at 60 DEG C, and as polyimides is titania-doped.
(5) 1.3g polyethylene terephthalate is dissolved in 18mL dehydrated alcohol, heating water bath is warming up to 55 DEG C, and stirring is extremely
It is completely dissolved, and is cooled to room temperature.
(6) the polyimides of step (4) is titania-doped, be added to step (5) have cooled to the poly- to benzene two of room temperature
In formic acid second diester, adjusting pH value with concentrated hydrochloric acid is 5.5, and ultrasonic disperse stirs 20min, makes polyimides is titania-doped to fill
Dispersion forms white suspension.
(7) the white suspension of step (6) is heated to 45 DEG C, reacts 30min.After reaction, it is cooled to room temperature,
Being neutralized to pH value with potassium hydroxide solution is 6.8.
(8) the solution of step (7) is filtered, 3.6h is dried in vacuo at 48 DEG C, and used after crushing to get giant electro-rheological liquid poly-
Ethylene terephthalate coats the titania-doped dielectric grain of polyimides.
(9) by polyethylene terephthalate cladding, polyimides is titania-doped is dispersed in amido silicon oil, gathers
It is 3g/mL, as giant electro-rheological liquid that ethylene terephthalate, which coats the titania-doped concentration of polyimides,；Through detecting,
The shear strength 39.4KPa (voltage 3kV) of the giant electro-rheological liquid, dynamic viscosity 91.3Pas (voltage 3kV, shear rate 100s-1), response time 3ms, room temperature sealing, which is placed 30 days, not to be settled.
Above-mentioned, although specific embodiments of the present invention have been described in conjunction with the embodiments, not protects to the present invention
The limitation of range, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art
The various modifications or changes that can be made are not needed to make the creative labor still within protection scope of the present invention.
Claims (7)
1. a kind of giant electro-rheological liquid dielectric grain, it is characterised in that: be nanometer core-shell structure composite material, with doping type two
Titanium oxide is core, and surface is coated with polar polymer；The doping type titanium dioxide is adulterated in titanium dioxide preparation process
High dielectric constant organic matter is prepared；Wherein, the mass fraction of titanium dioxide is 80%~90%, high dielectric constant organic matter
Mass fraction be 5%~10%, the mass fraction of polar polymer is 5%~10%；
The high dielectric constant organic matter is selected from one of Kynoar, polyvinyl fluoride, polyimides or a variety of；
The polar polymer is selected from one of polyacrylonitrile, polyethylene terephthalate, polyvinyl alcohol, polyaniline or more
Kind；
The preparation method of the giant electro-rheological liquid dielectric grain the following steps are included:
(1) 60~120mL titanate is dissolved in 60~120mL dehydrated alcohol, is denoted as A liquid；
(2) 0.6~1.6g high dielectric constant organic matter is dissolved in 10~20mL dehydrated alcohol, is denoted as B liquid；
(3) B liquid is added dropwise in A liquid, controls rate of titration in 0.17~0.35mL/min；Reaction is white to no longer generating
Precipitating, by the white precipitate washes of absolute alcohol of generation；
(4) white precipitate after above-mentioned cleaning is dried in vacuo 2~5h at 60~80 DEG C to get doping type titanium dioxide；
(5) 0.6~1.6g polar polymer is dissolved in 10~20mL dehydrated alcohol, obtains polar polymer solution；
(6) it by the doping type titanium dioxide of step (4), is added in the polar polymer solution of step (5), adjusting pH value is
4.0~5.5, ultrasonic disperse stirs 10~20min, is well dispersed in doping type titanium dioxide in polar polymer solution, shape
At white suspension；
(7) above-mentioned white suspension is heated to 45~60 DEG C, reacts 20~40min；After reaction, it is cooled to room temperature,
Adjusting pH value with alkaline solution is 6.8~7.2；
(8) solution of step (7) to be filtered, gained solid matter is dried in vacuo 2~4h at 40~50 DEG C after filtering, it crushes,
Up to giant electro-rheological liquid dielectric grain.
2. the preparation method of giant electro-rheological liquid dielectric grain according to claim 1, it is characterised in that: the step
(1) in, titanate is selected from one of isopropyl titanate, tetraisopropyl titanate, butyl titanate, positive four butyl ester of metatitanic acid, barium titanate
Or it is a variety of.
3. the preparation method of giant electro-rheological liquid dielectric grain according to claim 1, it is characterised in that: the step
(6) in, using concentrated hydrochloric acid or salt acid for adjusting pH value.
4. the preparation method of giant electro-rheological liquid dielectric grain according to claim 1, it is characterised in that: the step
(7) in, alkaline solution be selected from one of sodium hydroxide solution, potassium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution or
It is a variety of.
5. the preparation method of giant electro-rheological liquid dielectric grain according to any one of claims 1 to 4, feature exist
In: steps are as follows:
(1) 60mL isopropyl titanate is dissolved in 60mL dehydrated alcohol, stirs 30min at room temperature, obtained uniform solution and be denoted as A
Liquid；
(2) 1.0g polyvinyl fluoride is dissolved in 15mL dehydrated alcohol, stirs 20min at room temperature, obtained uniform solution and be denoted as B liquid；
(3) B liquid is added dropwise in A liquid, controls the rate of titration 0.25mL/min of solution；Reaction is heavy to white is no longer generated
It forms sediment, with washes of absolute alcohol, to remove the impurity in white precipitate；
By the white precipitate of step (3), it is dried in vacuo 2h at 80 DEG C, it is titania-doped to obtain polyvinyl fluoride；
1.5g polyaniline is dissolved in 15mL dehydrated alcohol, heating water bath is warming up to 55 DEG C, and stirring is and cooling to being completely dissolved
To room temperature；
By stepPolyvinyl fluoride it is titania-doped, be added to stepThe polyaniline solutions for having cooled to room temperature
In, adjusting pH value with concentrated hydrochloric acid is 4.5, and ultrasonic disperse stirs 18min, makes the titania-doped fully dispersed formation of polyvinyl fluoride
White suspension；
By stepWhite suspension be heated to 50 DEG C, react 20min；After reaction, it is cooled to room temperature, uses hydrogen-oxygen
Changing sodium solution to be neutralized to pH value is 7.1；
By stepSolution filtering, in 50 DEG C of vacuum drying 2h, after crushing to get.
6. the preparation method of giant electro-rheological liquid dielectric grain according to any one of claims 1 to 4, feature exist
In: steps are as follows:
(1) 100mL butyl titanate is dissolved in 100mL dehydrated alcohol, stirs 50min at room temperature, obtained uniform solution and be denoted as A
Liquid；
(2) 1.6g Kynoar is dissolved in 20mL dehydrated alcohol, stirs 30min at room temperature, obtained uniform solution and be denoted as B
Liquid；
(3) B liquid is added dropwise in A liquid, controls the rate of titration 0.35mL/min of solution；Reaction is heavy to white is no longer generated
It forms sediment, with washes of absolute alcohol, to remove the impurity in white precipitate；
By the white precipitate of step (3), 3h is dried in vacuo at 70 DEG C, as Kynoar is titania-doped；
1.3g polyacrylonitrile is dissolved in 15mL dehydrated alcohol, heating water bath is warming up to 50 DEG C, and stirring is and cold to being completely dissolved
But room temperature is arrived；
By stepKynoar it is titania-doped, be added to stepThe polyacrylonitrile for having cooled to room temperature
In solution, adjusting pH value with concentrated hydrochloric acid is 5.0, and ultrasonic disperse stirs 15min, makes Kynoar is titania-doped sufficiently to divide
It dissipates and forms white suspension；
By stepWhite suspension be heated to 60 DEG C, react 40min；After reaction, it is cooled to room temperature, uses carbonic acid
It is 7.0 that hydrogen sodium solution, which is neutralized to pH value,；
By stepSolution filtering, 3.5h is dried in vacuo at 45 DEG C, after crushing to get.
7. the preparation method of giant electro-rheological liquid dielectric grain according to any one of claims 1 to 4, feature exist
In: steps are as follows:
(1) positive four butyl ester of 120mL metatitanic acid is dissolved in 120mL dehydrated alcohol, stirs 60min at room temperature, obtain uniform solution note
For A liquid；
(2) 0.8g polyimides is dissolved in 12mL dehydrated alcohol, stirs 18min at room temperature, obtained uniform solution and be denoted as B liquid；
(3) B liquid is added dropwise in A liquid, controls the rate of titration 0.18mL/min of solution；Reaction is heavy to white is no longer generated
It forms sediment, with washes of absolute alcohol, to remove the impurity in white precipitate；
By the white precipitate of step (3), 5h is dried in vacuo at 60 DEG C, as polyimides is titania-doped；
1.3g polyethylene terephthalate is dissolved in 18mL dehydrated alcohol, heating water bath is warming up to 55 DEG C, stirs to complete
Dissolution, and it is cooled to room temperature；
By stepPolyimides it is titania-doped, be added to stepThe poly- terephthaldehyde for having cooled to room temperature
In sour second diester, adjusting pH value with concentrated hydrochloric acid is 5.5, and ultrasonic disperse stirs 20min, keeps polyimides titania-doped sufficiently
Dispersion forms white suspension；
By stepWhite suspension be heated to 45 DEG C, react 30min；After reaction, it is cooled to room temperature, uses
It is 6.8 that potassium hydroxide solution, which is neutralized to pH value,；
By stepSolution filtering, be dried in vacuo 3.6h at 48 DEG C, and after crushing to get.
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| KR20060015843A (en) * | 2004-08-16 | 2006-02-21 | 인하대학교 산학협력단 | An electrorheological fluid consisting of polyaniline/titanium dioxide composites as conducting particles and its preparation |
| JP2007065215A (en) * | 2005-08-30 | 2007-03-15 | Oji Paper Co Ltd | Display material and display device |
| CN1944606A (en) * | 2006-09-01 | 2007-04-11 | 中国科学院物理研究所 | Blended titanium dioxide electric rheological liquid and its preparing method |
| CN102108316A (en) * | 2009-12-23 | 2011-06-29 | 西北工业大学 | Titanium-oxide-coated polyaniline nanotube electrorheological fluid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20060015843A (en) * | 2004-08-16 | 2006-02-21 | 인하대학교 산학협력단 | An electrorheological fluid consisting of polyaniline/titanium dioxide composites as conducting particles and its preparation |
| JP2007065215A (en) * | 2005-08-30 | 2007-03-15 | Oji Paper Co Ltd | Display material and display device |
| CN1944606A (en) * | 2006-09-01 | 2007-04-11 | 中国科学院物理研究所 | Blended titanium dioxide electric rheological liquid and its preparing method |
| CN102108316A (en) * | 2009-12-23 | 2011-06-29 | 西北工业大学 | Titanium-oxide-coated polyaniline nanotube electrorheological fluid |
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