CN107393675A - A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO - Google Patents

A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO Download PDF

Info

Publication number
CN107393675A
CN107393675A CN201710572929.5A CN201710572929A CN107393675A CN 107393675 A CN107393675 A CN 107393675A CN 201710572929 A CN201710572929 A CN 201710572929A CN 107393675 A CN107393675 A CN 107393675A
Authority
CN
China
Prior art keywords
fluorine ether
acid
particle
magnetic
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710572929.5A
Other languages
Chinese (zh)
Inventor
陈芳
刘颖
颜招强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZIGONG ZHAOQIANG SEALING PRODUCT INDUSTRY Co Ltd
Sichuan University
Original Assignee
ZIGONG ZHAOQIANG SEALING PRODUCT INDUSTRY Co Ltd
Sichuan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ZIGONG ZHAOQIANG SEALING PRODUCT INDUSTRY Co Ltd, Sichuan University filed Critical ZIGONG ZHAOQIANG SEALING PRODUCT INDUSTRY Co Ltd
Priority to CN201710572929.5A priority Critical patent/CN107393675A/en
Publication of CN107393675A publication Critical patent/CN107393675A/en
Pending legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/447—Magnets 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Soft Magnetic Materials (AREA)
  • Lubricants (AREA)

Abstract

The present invention relates to novel intelligent fluent material and vibration damping, damping field, more particularly to a kind of preparation method of the compound fluorine ether oil based magnetic rheologic liquid of the high stability preparation methods that can be applied under the particular surroundings such as high/low temperature, acid and alkali corrosion are specially：Chemical coprecipitation is used to prepare Fe of the particle diameter for 5~15nm first3O4Nano particle；Then reacting liquid pH value is adjusted, nano magnetic particle is coated as surfactant using fluorine ether acid；A certain amount of graphene oxide water solution is added into reaction solution, ultrasound, stirring make particle and graphene sheet layer compound；Finally gained composite particles are distributed in fluorine ether oil, form fluorine ether acid@Fe3O4The compound fluorine ether oil based magnetic rheologic liquids [email protected] magnetic flow liquid has the fields such as property, the damping that is particularly suitable for use in, damping, Aero-Space, lubrication such as higher stability, low-friction coefficient, high saturation and magnetic intensity, corrosion-resistant, high-low temperature resistant.

Description

A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO
Technical field
The present invention relates to novel intelligent fluent material and vibration damping, damping field, more particularly to one kind can be in high/low temperature, soda acid The preparation method of the compound fluorine ether oil based magnetic rheologic liquid of high stability of application under the particular surroundings such as corrosion, specially a kind of fluorine ether Sour@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO.
Background technology
Magnetic flow liquid is a kind of novel intelligent fluent material, and carrier fluid is stably dispersed in by surfactant by magnetic-particle A kind of suspension of middle formation.When applying magnetic field, magnetic particles in fluid moment leads into chain or fibrous arrangement, this arrangement Fluid viscosity increase is caused, mobility reduces and shows obvious solid property；When magnetic field disappears, magnetic particles in fluid recovers To original free disordered state, mobility is also recovered therewith.Magnetic flow liquid because having unique physicochemical property under magnetic field and Receive significant attention.Magnetic rheology effect is found from Rabinow in 1948 so far, and the technology has had to develop on a large scale very much, in aviation Many fields such as space flight, electronics, chemical industry, the energy are applied, especially in damper, brake valve, clutch, magnetorheological damping Etc. application it is ripe.
The conventional magnetic-particle of magnetic flow liquid belongs to metallic particles, such as Co, Ni, carbonyl iron dust, has larger density, And the density of carrier fluid is relatively small, this will cause magnetic-particle to be easy to be deposited in bottom.The stability of magnetic flow liquid is to judge The very important index of magnetorheological fluid performance, also directly determines its application effect.To lift the stability of magnetic flow liquid, patent CN 104673475 A reduce the density of particle, lifting particle dispersion by adding graphene oxide, prepare stable water base magnetic Rheology liquid.Graphene oxide is attached to carbonyl iron particles top layer by W.L.Zhang and H.J.Choi, reduces grain density, lifting Magnetic flow liquid stability., it is necessary to high-low temperature resistant, corrosion-resistant, high stability, high saturation in the application of some special industry environment The magnetic flow liquid of the performances such as the intensity of magnetization, therefore, it is necessary to further lift magnetic flow liquid species and performance.
The content of the invention
The goal of the invention of the present invention is to be directed to above technical problem, there is provided a kind of fluorine ether acid@Fe3O4The compound fluorine ether oil bases of@GO The preparation method of magnetic flow liquid.The fluorine ether acid@Fe prepared using this method3O4The compound fluorine ether oil based magnetic rheologic liquids of@GO can solve Existing magnetic flow liquid free settling and the problem of can not be used under special operation condition.
The present invention concrete technical scheme be：
A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, wherein magnetic flow liquid include compound Nano magnetic particle and base load liquid.
Above-mentioned composite Nano magnetic-particle is fluorine ether acid@Fe3O4@GO, Fe is prepared using chemical coprecipitation first3O4Receive Rice grain, particle diameter are 5~15nm.Fe is coated with fluorine ether acid Surfactant Chemistry3O4Nano magnetic particle, then make particle with Graphene oxide is compound.The cladding of fluorine ether acid is in order to avoid particle is oxidized while promotes the compatibility of particle and base load liquid. Graphene oxide is in order to lift the dispersiveness of particle, so as to prepare high stability magnetic flow liquid.Above-mentioned base load liquid is fluorine ether oil, With the performance such as high-low temperature resistant, corrosion-resistant, by fluorine ether acid@Fe3O4@GO composite particles are scattered in fluorine ether oil, and preparation can be applied to High stability fluorine ether oil based magnetic rheologic liquid under special extreme environment.
A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, concrete operations are as follows：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1 by mol ratio:1~2:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, temperature 70 ℃.Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution prepared is rapidly added extremely Reacting liquid pH value is more than 10, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Then Watery hydrochloric acid is added dropwise into reaction solution, adjusts its pH value as 6~8.Surfactant fluorine 2~6g of ether acid is added into reaction solution again, 2h is stirred with 500r/min speed mechanical.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 100mL graphene oxide water solutions (mass fraction ω=0.5%) ultrasonic disperse 30min, add mixed obtained by (2) Close in liquid, mechanical agitation 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone. Magneto separate removes moisture content in mixed liquor, and colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
To be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle be 30%~ 70%, ultrasound, stirring 4h, mixing speed 500r/min, high stability fluorine ether acid@Fe are made3O4The compound fluorine ether oil magnetic currents of@GO Become liquid.
The positive effect of the present invention is embodied in：
Fluorine ether acid@Fe prepared by the present invention3O4The compound fluorine ether oil based magnetic rheologic liquids of@GO have good stability, can apply In hot environment, corrosive atmosphere operating mode, the performance of magnetic flow liquid is lifted, widens its application.
Brief description of the drawings
Fig. 1 is fluorine ether acid@Fe3O4The XRD of@GO composite particles；30.5 ° (220) are can be seen that from XRD, 35.7 ° (311), 43.2 ° (400), 53.7 ° (422), 57 ° (511), 62.8 ° (440), 75 ° (533), with PDF card 03-0863 peak values Unanimously, composite particles are inverse spinel structure, illustrate that fluorine ether acid has no effect on its lattice types to the cladding of magnetic-particle.GO's Comparision contents are few, and peak value is very weak to be embodied, and particle lattice type is not had an impact.
Fig. 2 is fluorine ether acid@Fe3O4The scanning electron microscope (SEM) photograph of@GO composite particles；From SEM it can be seen from the figure thats, countless particles are attached And be grown in graphene oxide layer, illustrate that graphene oxide layer is combined very well with particle；Grain diameter size is about 5~ 15nm。
Fig. 3 is fluorine ether acid@Fe3O4The hysteresis graph of@GO composite particles；From VSM it can be seen from the figure thats, composite particles tool There is less coercivity can be neglected, superparamagnetism is presented, there is higher specific saturation magnetization 45.26emu/g.
Fig. 4 is fluorine ether acid@Fe3O4The infrared spectrogram of@GO composite particles；From FT-IR it can be seen from the figure thats, 584.6cm-1 The corresponding Fe in place3O4The stretching vibration peak of middle Fe-O keys.3421.8cm-1And 1677.7cm-1Place is that O-H flexible and deformation is shaken respectively Dynamic peak, certain moisture content is adsorbed for particle surface.983cm-1Place is C-O-C stretching vibration peak, 1240,1190 and 1306cm-1Place be respectively C-F keys, F-C-F keys,The stretching vibration peak of key, 1712cm-1Place is the stretching vibration of C=O keys Peak, show fluorine ether acid chemisorbed in Fe3O4Particle top layer.
Fig. 5 is fluorine ether acid@Fe3O4The compound magnetic flow liquids of@GO apply the intuitive manner before and after magnetic field；Contrast can be with from figure Find out, the magnetic flow liquid has good magnetic responsiveness.
Embodiment
With reference to embodiment, the present invention is further described, but does not limit the scope of the invention.
Embodiment 1:
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.69 by mol ratio：1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Then to anti- Answer and watery hydrochloric acid is added dropwise in liquid, adjust its pH value as 6.48.Surfactant fluorine ether acid 2g is added into reaction solution again, with 500r/ Min speed mechanical stirring 2h.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 100mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), Mechanical agitation 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate is gone Except moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 70%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquids of@GO, saturated magnetization are strong The higher 24.5emu/g of degree, the magnetic flow liquid stability is fine, and centrifugation does not find agglomerated particle.The magnetorheological fluid performance is superior, long Damping damping for being applied to acid and alkali corrosion environment, high and low temperature environment of phase stabilization etc..
Embodiment 2：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.72 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Then to anti- Answer and watery hydrochloric acid is added dropwise in liquid, adjust its pH value as 6.39.Surfactant fluorine ether acid 3g is added into reaction solution again, with 500r/ Min speed mechanical stirring 2h.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 80mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), machine Tool stirs 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate removes Moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 60%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made high stability fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquids of@GO, satisfy With the higher 21.6emu/g of the intensity of magnetization, centrifugation finds no larger particles appearance, the application that the magnetic flow liquid can be steady in a long-term Damped in the damping of acid and alkali corrosion environment, high and low temperature environment etc..
Embodiment 3：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 3.9 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C.It is real Rare gas is continually fed into during testing.After mechanical agitation makes grain dissolution, it is rapidly added the NaOH aqueous solution prepared and extremely reacts Liquid pH value is 11, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Then to reaction Watery hydrochloric acid is added dropwise in liquid, it is about 6.15 to adjust its pH value.Surfactant fluorine ether acid 2g is added into reaction solution again, with 500r/ Min speed mechanical stirring 2h.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 100mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), Mechanical agitation 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate is gone Except moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 70%, is surpassed Sound, stirring 4h, mixing speed 500r/min, it is brownish red that fluorine ether oil magnetic flow liquid color, which is made, relatively stable, but saturated magnetization The relatively low about 11.1emu/g of intensity, is unfavorable for the application of damping damping.
Embodiment 4：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.66 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Regulation reaction Liquid pH value is 6.52, adds surfactant fluorine ether acid 10g, and 2h is stirred with 500r/min speed mechanical.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 100mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), Mechanical agitation 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate is gone Except moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 30%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquids of@GO, black is presented, surely Qualitative preferable, the higher about 17.5emu/g of saturation magnetization, slightly relatively low, the magnetic flow liquid can be applied to its saturated magnetization Intensity meter requires relatively low high and low temperature environment, acid and alkali corrosion environment.
Embodiment 5：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.93 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Regulation reaction Liquid pH value is 10.86, adds surfactant fluorine ether acid 2g, and 2h is stirred with 500r/min speed mechanical.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 80mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), machine Tool stirs 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate removes Moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 70%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquid saturation magnetizations of@GO About 25.3emu/g, less stable, centrifugation find that many particles settle, the inclined brownish red of color of magnetic flow liquid.The magnetic Rheology liquid is unsuitable for actual damping, damping application.
Embodiment 6：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.71 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Regulation reaction Liquid pH value is 6.23, adds surfactant fluorine ether acid 3g, and 2h is stirred with 500r/min speed mechanical.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 500mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), Mechanical agitation 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate is gone Except moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 50%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquids of@GO, black is presented, satisfies There is larger piece Rotating fields thing with the higher about 19.0emu/g of the intensity of magnetization, less stable, centrifugation, it is impossible to application well In compared with high and low temperature environment, acid and alkali corrosion environment.
Embodiment 7：
(1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
It is 1.75 by mol ratio:1 Fe3+And Fe2+Salt is placed in 70 DEG C of ultra-pure water, heating water bath, and temperature is 70 DEG C. Rare gas is continually fed into experimentation.After mechanical agitation makes grain dissolution, the NaOH aqueous solution for preparing is rapidly added to anti- It is 11 to answer liquid pH value, while carries out intense mechanical stirring, mixing speed 500r/min, reaction time 30min.Regulation reaction Liquid pH value is 6.34, adds surfactant fluorine ether acid 2g, and 2h is stirred with 500r/min speed mechanical.
(2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
To 50mL graphene oxide water solutions (ω=0.5%) ultrasonic disperse 30min, add in mixed liquor obtained by (2), machine Tool stirs 2h, mixing speed 500r/min.Particle is cleaned to reacting liquid pH value close to 7 with ultra-pure water, acetone.Magneto separate removes Moisture content in mixed liquor, colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h.
(3) particle is scattered
It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 10%, is surpassed Sound, stirring 4h, mixing speed 500r/min, are made fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquid stability of@GO is preferable, The non-particle of centrifugation settles, but its saturation magnetization is too low, about 4.9emu/g, can be only applied to satisfy to magnetic flow liquid The not high application environment with the intensity of magnetization.
Above-described embodiment overview is as shown in the table,
Embodiment is just to clear explanation example of the present invention, not to the restriction of embodiment.For this public affairs For those of ordinary skill belonging to department, various forms of changes or change can also be made on the basis of the above description, by This obvious changes or variations extended out is within protection scope of the present invention.

Claims (7)

  1. A kind of 1. fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, it is characterised in that including following step Suddenly：
    A. fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle：Use chemical coprecipitation prepare particle diameter for 5~ 15nm Fe3O4Magnetic-particle, the pH value of reaction solution is then adjusted, with fluorine ether acid chemistry coated particle；
    B. fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles：The graphene oxide that ultrasonic disperse is added into reaction solution is water-soluble Liquid, mechanical agitation make nano particle compound with graphene sheet layer, form fluorine ether acid@Fe3O4@GO composite particles；
    C. particle is scattered：Composite particles mechanical agitation is distributed in fluorine ether oil, forms fluorine ether acid@Fe3O4The compound fluorine ethers of@GO Oil base magnetic flow liquid.
  2. A kind of 2. fluorine ether acid@Fe according to claim 13O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, its It is characterised by：In described step A, after particles generation, the pH value for adjusting reaction solution is 6~8, adds 2~6g of fluorine ether acid.
  3. A kind of 3. fluorine ether acid@Fe according to claim 13O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, its It is characterised by：In described step B, it is that 0.5% graphene oxide water solution carries out ultrasonic disperse by mass fraction, obtains uniformly Graphene solution, 50~100ml is then added into step B resulting solutions, mechanical agitation 2h prepares fluorine ether acid@Fe3O4@GO Composite particles.
  4. A kind of 4. fluorine ether acid@Fe according to claim 13O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, its It is characterised by：Composite particles account for magnetic flow liquid mass ratio as 30%~80%.
  5. A kind of 5. fluorine ether acid@Fe according to claim 13O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, its The structural formula for being characterised by PFPE carboxylic acid is：Wherein n=4~35.
  6. A kind of 6. fluorine ether acid@Fe according to claim 13O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO, its The structural formula for being characterised by perfluoro polyether oil is：Wherein n=1~60.
  7. A kind of 7. fluorine ether acid@Fe according to any one claim in claim 1-63O4The compound fluorine ether oil base magnetic currents of@GO Become the preparation method of liquid, it is characterised in that specifically include following steps：
    (1) fluorine ether acid@Fe3O4The preparation of high saturation and magnetic intensity nano particle
    It is 1 by mol ratio:1~2:1 Fe3+And Fe2+Salt is placed in heating water bath in ultra-pure water, and temperature is 70 DEG C；In experimentation Rare gas is continually fed into, after mechanical agitation makes grain dissolution, it is big to reacting liquid pH value to be rapidly added the NaOH aqueous solution prepared In 10, while intense mechanical stirring is carried out, mixing speed 500r/min, reaction time 30min；Then dripped into reaction solution Add watery hydrochloric acid, adjust its pH value as 6~8；Surfactant fluorine 2~6g of ether acid is added into reaction solution again, with 500r/min's Speed mechanical stirs 2h；
    (2) fluorine ether acid@Fe3O4The preparation of@GO composite magnetic particles
    Ultrasonic disperse 30min is carried out to 100mL (mass fraction is ω=0.5%) graphene oxide water solution, adds (1) institute Obtain in mixed liquor, mechanical agitation 2h, mixing speed 500r/min；Particle to reacting liquid pH value is cleaned with ultra-pure water, acetone to connect Nearly 7；Magneto separate removes moisture content in mixed liquor, and colloidal solid is placed in 70 DEG C of vacuum drying chambers and dries more than 10h；
    (3) particle is scattered
    It will be scattered in after composite particles grinding obtained by (2) in fluorine ether oil base fluid, wherein mass ratio shared by particle is 30%~70%, Ultrasound, stirring 4h, mixing speed 500r/min, are made high stability fluorine ether acid@Fe3O4The compound fluorine ether oil magnetic flow liquids of@GO.
CN201710572929.5A 2017-07-14 2017-07-14 A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO Pending CN107393675A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710572929.5A CN107393675A (en) 2017-07-14 2017-07-14 A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710572929.5A CN107393675A (en) 2017-07-14 2017-07-14 A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO

Publications (1)

Publication Number Publication Date
CN107393675A true CN107393675A (en) 2017-11-24

Family

ID=60340129

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710572929.5A Pending CN107393675A (en) 2017-07-14 2017-07-14 A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO

Country Status (1)

Country Link
CN (1) CN107393675A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103337329A (en) * 2013-07-11 2013-10-02 江苏海纳磁性纳米新材料科技有限公司 Preparing method of perfluoroalkylpolyether oil-based magnetofluid
CN103680798A (en) * 2013-12-17 2014-03-26 北京交通大学 Preparation method for perfluor polyether oil-based magnetic liquid
CN103996480A (en) * 2014-06-11 2014-08-20 黑龙江工程学院 Perfluoropolyether-grease-based magnetic fluid and preparation method thereof
CN104673475A (en) * 2015-02-16 2015-06-03 中北大学 Graphene @Fe3O4 compound water base magnetorheological fluid and preparation method thereof
CN106410426A (en) * 2016-11-25 2017-02-15 东莞市联洲知识产权运营管理有限公司 Silicon oil magnetic fluid absorbing material based on carboxy siloxane and preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103337329A (en) * 2013-07-11 2013-10-02 江苏海纳磁性纳米新材料科技有限公司 Preparing method of perfluoroalkylpolyether oil-based magnetofluid
CN103680798A (en) * 2013-12-17 2014-03-26 北京交通大学 Preparation method for perfluor polyether oil-based magnetic liquid
CN103996480A (en) * 2014-06-11 2014-08-20 黑龙江工程学院 Perfluoropolyether-grease-based magnetic fluid and preparation method thereof
CN104673475A (en) * 2015-02-16 2015-06-03 中北大学 Graphene @Fe3O4 compound water base magnetorheological fluid and preparation method thereof
CN106410426A (en) * 2016-11-25 2017-02-15 东莞市联洲知识产权运营管理有限公司 Silicon oil magnetic fluid absorbing material based on carboxy siloxane and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SHARAFELDIN M,ET AL: "Fe3O4 nanoparticles on graphene oxide sheets for isolation and ultrasensitive amperometric detection of cancer biomarker proteins", 《BIOSENSORS & BIOELECTRONICS》 *

Similar Documents

Publication Publication Date Title
CN105143109B (en) Ferric oxide nano magnetic-particle powder and its manufacture method, the ferric oxide nano magnetic granular thin film comprising the ferric oxide nano magnetic-particle powder and its manufacture method
Yu et al. Study of preparation and properties on magnetization and stability for ferromagnetic fluids
CN1230501C (en) Stable magnetic rheological liquid and its preparation method
JP4749733B2 (en) Hydrophobic magnetic iron oxide particles
TW201135760A (en) Ferromagnetic particle powder and manufacturing method thereof, and anisotropic magnet and bonded magnet
Sun et al. Magnetic separation of polymer hybrid iron oxide nanoparticles triggered by temperature
CN109665565B (en) Nano Fe3O4Preparation method of composite graphene and nano Fe3O4Composite graphene
CN101599335A (en) A kind of oxidation resistant dimethyl silicon oil based magnetic fluid and preparation method thereof
Cao et al. Green synthesis and surface properties of Fe3O4@ SA core–shell nanocomposites
CN108704610A (en) The Mg-Fe ball composite material and preparation method of magnetic carbon modification and application
Chen et al. Size effect of Fe3O4 nanoparticles on magnetism and dispersion stability of magnetic nanofluid
CN106548847A (en) A kind of magnetic flow liquid and preparation method thereof
Zheng et al. High performance shear thickening fluid based on calcinated colloidal silica microspheres
Sun et al. Effect of MXene nanosheets attached to carbonyl iron microspheres on the performance and stability of magnetorheological fluid
Zhang et al. Self-assembly of graphene oxide coated soft magnetic carbonyl iron particles and their magnetorheology
CN111517372A (en) Fullerene coated Fe3O4Composite nano material and preparation method thereof
Yang et al. Fabrication, mechanical, and electromagnetic studies of cobalt ferrite based‐epoxy nanocomposites
CN107393675A (en) A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO
CN102728275B (en) Preparation method of hydrophobic magnetic powder
CN113972061B (en) Preparation method of magnetorheological fluid with high dispersion stability
CN111233046A (en) Hollow magnetic Fe for magnetorheological fluid3O4Nano-doped microsphere and preparation method thereof
CN110935405B (en) Preparation method of magnetic polystyrene microspheres with surfaces rich in double bonds
CN110614082B (en) Carbon black-superparamagnetic Fe3O4Preparation and application of nano-composite
CN109065319A (en) A kind of superelevation saturation magnetization Fe3O4The preparation method of nano particle and its magnetic fluid
JP2017183322A (en) Bond magnet arranged by use of iron nitride-based magnetic powder

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20171124