CN107418210A - A kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber - Google Patents

A kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber Download PDF

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Publication number
CN107418210A
CN107418210A CN201710424347.2A CN201710424347A CN107418210A CN 107418210 A CN107418210 A CN 107418210A CN 201710424347 A CN201710424347 A CN 201710424347A CN 107418210 A CN107418210 A CN 107418210A
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silicone rubber
elastomer based
stirred
magnetorheological elastomer
rheomagnetic
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陈刚
王艳芹
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Changzhou Ruitai Materials Co Ltd
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Changzhou Ruitai Materials Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/447Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids characterised by magnetoviscosity, e.g. magnetorheological, magnetothixotropic, magnetodilatant liquids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0856Iron
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives

Abstract

The invention discloses a kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber, belong to magnetorheological materials field.The present invention is dissolved in water by ironic citrate and ferric nitrate, with graphite oxide composite drying and calcination processing, then with carbonyl iron dust composite ball-milling and being mixed with liquid silastic, shear and ultrasonic disperse is handled, it is prepared into conducting liquid silicon rubber, then silicon rubber energization is handled, it is set to produce magnetic field, carbonyl iron dust and ferrite powder are produced to the distribution for complying with magnetic field, finally stand solidification and be prepared into high rheological variation elastomer, high magnetic current modification magnetorheological elastomer based on silicone rubber prepared by the present invention is by improving the difference of internal magnetization particle, greatly enhance magnetic rheology effect, and by preparing equally distributed magnetorheological elastomer based on silicone rubber, it greatly strengthen the tensile strength and rebound performance of silicon rubber, safe preparation process green, it is pollution-free.

Description

A kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber
Technical field
The invention discloses a kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber, belong to magnetorheological material Material field.
Background technology
Magnetorheological materials are a kind of new intellectual materials of recent decades development, because it has a kind of special physics Effect --- magnetic rheology effect, magnetorheological materials are the new function materials that a kind of mechanical property can be controlled by magnetic field.Due to it Have the characteristics that fast response, good reversibility and the mechanical properties by adjusting the controllable prepared material of magnetic field size change, because And it is obtained for extensive use in fields such as building, automobile, vibration controls in recent years.Magnetic rheology elastic body is magnetorheological materials man A new member in race.It is to be blended in polymeric matrix material and solidify shape micron or nano level ferromagnetic particle Into, polymer of the mixing with ferromagnetic particle applies externally-applied magnetic field in the curing process, using magnetic rheology effect, makes matrix In ferromagnetic particle chain or column structure are formed on magnetic direction.
In addition to the mechanical property with field controllable, the other performance of magnetic rheology elastic body can also be controlled by magnetic field, Such as damping capacity, rigidity, magnetic property etc..These special performances cause magnetic rheology elastic body to have broad application prospects.But Be the magnetic rheology elastic body prepared at present due to a lack of larger magnetic rheology effect, limit their extensive uses industrially. When magnetic-particle is identical, the relative magnetic rheology effect that the softer flexible base material of use can improve magnetic rheology elastic body is right And it is relatively low as the magnetorheological elastomer material mechanical strength of matrix using silicon rubber, gel, polyurethane, fatigue resistance is poor, is not suitable for Application in terms of most of load-bearing, although while existing magnetic-particle dispersiveness preferably, its skewness, not only lead Cause composite elastic body mechanical property poor, also reduce elastomer rheomagnetic energy, its use range is influenceed, so preparing a kind of power It is particularly important to learn the good high rheomagnetic magnetorheological elastomer based on silicone rubber of performance.
The content of the invention
Present invention mainly solves technical problem:For existing magnetorheological elastomer based on silicone rubber skewness, not only Cause composite elastic body mechanical property poor, also reduce elastomer rheomagnetic energy, the problem of influenceing its use range, there is provided A kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)In mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred to obtain iron ion mixed liquor with deionized water, by matter Measure ratio 1:5,100 mesh graphite oxides are stirred with iron ion mixed liquor, still aging and dry drying crystalline, by drying Crystallization is calcined and is cooled to room temperature, obtains calcining particle, in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, ball milling 200 mesh sieves are crossed, obtain mixing and ball milling powder;
(2)In mass ratio 1:8, mixing and ball milling powder and liquid silastic LSR are stirred and are placed in high-speed shearing machine, is cut Processing and 10~15min of ultrasonic disperse are cut, mixed dispersion liquid is obtained, takes 500~600mL mixed dispersion liquids to be placed in tank, by two Block graphite cake is placed in parallel and immersed in mixed dispersion liquid, and switch on power two-stage, is powered and handles and stand solidification, completion to be solidified After remove voltage, you can be prepared into a kind of high rheomagnetic magnetorheological elastomer based on silicone rubber.
Step(2)To apply 25kHz pulse current, pulse amplitude 20V, current density is for described energization processing 10mA/cm2
The beneficial effects of the invention are as follows:
The present invention is doped into liquid silastic by iron oxide, graphite and carbonyl iron dust, prepares conductivity type liquid silastic, then It is dissolved in water by ironic citrate and ferric nitrate, with graphite oxide composite drying and calcination processing, is then answered with carbonyl iron dust Close ball milling and mixed with liquid silastic, shear and ultrasonic disperse is handled, conducting liquid silicon rubber is prepared into, then to silicon rubber Energization is handled, and it is produced magnetic field, because carbonyl iron dust is acted on forming equally distributed structure by field strength, is made magnetic rheology elastic body It is evenly distributed, improves magnetic rheology elastic body rheological property, carbonyl iron dust and ferrite powder produces the distribution for complying with magnetic field, finally Stand solidification and be prepared into high rheological variation elastomer, improve the distribution of internal magnetization particle, greatly enhance magnetic rheology effect.
Embodiment
First in mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred with deionized water, at 45~50 DEG C After mixing 15~20min, iron ion mixed liquor is prepared into, then in mass ratio 1:5, by 100 mesh graphite oxides stirring with iron from Sub- mixed liquor is stirred 25~30min, after subsequent still aging 3~5h, then 6~8h is dried at 65~70 DEG C;It is to be dried After the completion of, obtain drying crystalline and be placed in crucible, 550~600 DEG C, after 1~2h is calcined in insulation are heated to by 10 DEG C/min heatings Standing is cooled to room temperature, obtains calcining particle and in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, then 350~ 2~3h of ball milling under 400r/min, cross 200 mesh sieves and obtain mixing and ball milling powder;In mass ratio 1:8, by mixing and ball milling powder and liquid Silicon rubber LSR, which is stirred, to be placed in high-speed shearing machine, after 25~30min of shear treatment, the ultrasonic disperse under 200~300W 10~15min, obtain mixed dispersion liquid;500~600mL mixed dispersion liquids are taken to be placed in tank, by two pieces of 50mm × 50mm × 5mm Graphite cake be placed in parallel and immerse in mixed dispersion liquid, switch on power two-stage, applies 25kHz pulse current, pulse to it Amplitude is 20V, current density 10mA/cm2, subsequently power on and stand 10~12h of solidification, voltage is removed after the completion of to be solidified simultaneously Stand 45~60min, you can be prepared into a kind of high magnetic current modification magnetorheological elastomer based on silicone rubber.
Example 1
First in mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred with deionized water, 15min is mixed at 45 DEG C Afterwards, iron ion mixed liquor is prepared into, then in mass ratio 1:5, the stirring of 100 mesh graphite oxides is stirred with iron ion mixed liquor and mixed 25min is closed, then after still aging 3h, then 6h is dried at 65 DEG C;After the completion of to be dried, obtain drying crystalline and be placed in crucible In, it is heated to 550 DEG C by 10 DEG C/min heatings, is stood after insulation calcining 1h and be cooled to room temperature, obtains calcining particle and in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, then the ball milling 2h under 350r/min, cross 200 mesh sieves and obtain mixing and ball milling powder End;In mass ratio 1:8, mixing and ball milling powder and liquid silastic LSR are stirred and are placed in high-speed shearing machine, at shearing After managing 25min, ultrasonic disperse 10min, obtains mixed dispersion liquid under 200W;500mL mixed dispersion liquids are taken to be placed in tank, by two Block 50mm × 50mm × 5mm graphite cake is placed in parallel and immersed in mixed dispersion liquid, and switch on power two-stage, and it is applied 25kHz pulse current, pulse amplitude 20V, current density 10mA/cm2, subsequently power on and stand solidification 10h, it is to be solidified After the completion of remove voltage and stand 45min, you can be prepared into a kind of high magnetic current modification magnetorheological elastomer based on silicone rubber.
Example 2
First in mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred with deionized water, 18min is mixed at 48 DEG C Afterwards, iron ion mixed liquor is prepared into, then in mass ratio 1:5, the stirring of 100 mesh graphite oxides is stirred with iron ion mixed liquor and mixed 28min is closed, then after still aging 4h, then 7h is dried at 68 DEG C;After the completion of to be dried, obtain drying crystalline and be placed in crucible In, it is heated to 580 DEG C by 10 DEG C/min heatings, is stood after insulation calcining 2h and be cooled to room temperature, obtains calcining particle and in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, then the ball milling 3h under 380r/min, cross 200 mesh sieves and obtain mixing and ball milling powder End;In mass ratio 1:8, mixing and ball milling powder and liquid silastic LSR are stirred and are placed in high-speed shearing machine, at shearing After managing 28min, ultrasonic disperse 13min, obtains mixed dispersion liquid under 250W;550mL mixed dispersion liquids are taken to be placed in tank, by two Block 50mm × 50mm × 5mm graphite cake is placed in parallel and immersed in mixed dispersion liquid, and switch on power two-stage, and it is applied 25kHz pulse current, pulse amplitude 20V, current density 10mA/cm2, subsequently power on and stand solidification 11h, it is to be solidified After the completion of remove voltage and stand 52min, you can be prepared into a kind of high magnetic current modification magnetorheological elastomer based on silicone rubber.
Example 3
First in mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred with deionized water, 20min is mixed at 50 DEG C Afterwards, iron ion mixed liquor is prepared into, then in mass ratio 1:5, the stirring of 100 mesh graphite oxides is stirred with iron ion mixed liquor and mixed 30min is closed, then after still aging 5h, then 8h is dried at 70 DEG C;After the completion of to be dried, obtain drying crystalline and be placed in crucible In, it is heated to 600 DEG C by 10 DEG C/min heatings, is stood after insulation calcining 2h and be cooled to room temperature, obtains calcining particle and in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, then the ball milling 3h under 400r/min, cross 200 mesh sieves and obtain mixing and ball milling powder End;In mass ratio 1:8, mixing and ball milling powder and liquid silastic LSR are stirred and are placed in high-speed shearing machine, at shearing After managing 30min, ultrasonic disperse 15min, obtains mixed dispersion liquid under 300W;600mL mixed dispersion liquids are taken to be placed in tank, by two Block 50mm × 50mm × 5mm graphite cake is placed in parallel and immersed in mixed dispersion liquid, and switch on power two-stage, and it is applied 25kHz pulse current, pulse amplitude 20V, current density 10mA/cm2, subsequently power on and stand solidification 12h, it is to be solidified After the completion of remove voltage and stand 60min, you can be prepared into a kind of high magnetic current modification magnetorheological elastomer based on silicone rubber.
By high magnetic current modification magnetorheological elastomer based on silicone rubber obtained by above-described embodiment and conventional silicone rubber based magnetic rheologic bullet Property body is detected, and is contrasted, as a result as shown in Table 1.
Table one:
Remarks:1# is conventional silicone rubber based magnetic rheologic elastomer.
As seen from the above table, the high magnetic current modification magnetorheological elastomer based on silicone rubber of the present invention has preferable mechanical property and magnetic Rheological property, tensile strength are 11.5~12.7MPa, and rebound degree is 58~62%, and hardness is 45~48A, and magnetic rheology effect is significantly Enhancing, up to 70~81%, magneto-induced modulus is up to 1.35~1.48MPa.

Claims (2)

1. a kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber, it is characterised in that specifically preparation process is:
(1)In mass ratio 1:1:10, ironic citrate and ferric nitrate are stirred to obtain iron ion mixed liquor with deionized water, by matter Measure ratio 1:5,100 mesh graphite oxides are stirred with iron ion mixed liquor, still aging and dry drying crystalline, by drying Crystallization is calcined and is cooled to room temperature, obtains calcining particle, in mass ratio 1:5, calcining particle and carbonyl iron dust are stirred, ball milling 200 mesh sieves are crossed, obtain mixing and ball milling powder;
(2)In mass ratio 1:8, mixing and ball milling powder and liquid silastic LSR are stirred and are placed in high-speed shearing machine, is cut Processing and 10~15min of ultrasonic disperse are cut, mixed dispersion liquid is obtained, takes 500~600mL mixed dispersion liquids to be placed in tank, by two Block graphite cake is placed in parallel and immersed in mixed dispersion liquid, and switch on power two-stage, is powered and handles and stand solidification, completion to be solidified After remove voltage, you can be prepared into a kind of high rheomagnetic magnetorheological elastomer based on silicone rubber.
2. a kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber according to claim 1, its feature It is:Step(2)Described energization processing is to apply 25kHz pulse current, pulse amplitude 20V, current density 10mA/ cm2
CN201710424347.2A 2017-06-07 2017-06-07 A kind of preparation method of high rheomagnetic magnetorheological elastomer based on silicone rubber Withdrawn CN107418210A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110862689A (en) * 2019-11-29 2020-03-06 中国科学院合肥物质科学研究院 Preparation method of magnetic control flexible surface material with orthotropic wettability
CN113583448A (en) * 2021-08-25 2021-11-02 中国科学院宁波材料技术与工程研究所 Deformable-variable-rigidity dual-function magnetic intelligent material and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101740192A (en) * 2009-12-24 2010-06-16 上海交通大学 Thermoplastic magnetorheological elastomer composite material and preparation method thereof
CN102675668A (en) * 2012-05-30 2012-09-19 电子科技大学 Preparation method for nanoparticle magnetorheological elastomer thin film
CN103435822A (en) * 2013-07-05 2013-12-11 西南交通大学 Method for preparing magnetorheological elastomer by using pulsating magnetic field
CN104788938A (en) * 2015-04-13 2015-07-22 重庆大学 High-damping and high-strength magneto-rheological elastomer and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101740192A (en) * 2009-12-24 2010-06-16 上海交通大学 Thermoplastic magnetorheological elastomer composite material and preparation method thereof
CN102675668A (en) * 2012-05-30 2012-09-19 电子科技大学 Preparation method for nanoparticle magnetorheological elastomer thin film
CN103435822A (en) * 2013-07-05 2013-12-11 西南交通大学 Method for preparing magnetorheological elastomer by using pulsating magnetic field
CN104788938A (en) * 2015-04-13 2015-07-22 重庆大学 High-damping and high-strength magneto-rheological elastomer and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110862689A (en) * 2019-11-29 2020-03-06 中国科学院合肥物质科学研究院 Preparation method of magnetic control flexible surface material with orthotropic wettability
CN110862689B (en) * 2019-11-29 2022-04-26 中国科学院合肥物质科学研究院 Preparation method of magnetic control flexible surface material with orthotropic wettability
CN113583448A (en) * 2021-08-25 2021-11-02 中国科学院宁波材料技术与工程研究所 Deformable-variable-rigidity dual-function magnetic intelligent material and preparation method and application thereof

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