CN105225786A - A kind of preparation method of PFPE oil-based magnetic fluids material - Google Patents

A kind of preparation method of PFPE oil-based magnetic fluids material Download PDF

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Publication number
CN105225786A
CN105225786A CN201510729740.3A CN201510729740A CN105225786A CN 105225786 A CN105225786 A CN 105225786A CN 201510729740 A CN201510729740 A CN 201510729740A CN 105225786 A CN105225786 A CN 105225786A
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Prior art keywords
pfpe oil
based magnetic
surfactant
transition liquid
preparation
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CN201510729740.3A
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杨阳
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JIANGSU HINANO PRECISION ASSEMBLY Co Ltd
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JIANGSU HINANO PRECISION ASSEMBLY Co Ltd
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Publication of CN105225786A publication Critical patent/CN105225786A/en
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Abstract

The invention discloses a kind of preparation method of PFPE oil-based magnetic fluids material, belong to material and preparing technical field thereof.Described PFPE oil-based magnetic fluids material utilizes precipitation method synthesis of nano magnetic particles of ferroferric oxide; while synthesis, utilize fluorine ether surfactant to modify; then with water and alcohol alternately cleaning; the magnetic particle obtained can be dispersed in transition liquid; transition liquid is finally utilized aid dispersion surfactant, carrier fluid and magnetic particle to be dissolved each other; in the process of heating, remove transition liquid, obtain the PFPE oil-based magnetic fluids that dispersion effect is good.PFPE oil-based magnetic fluids of the present invention is applicable to dynamic vacuum sealing, can meet harsh super quiet, hot environment, has the good characteristic of waterproof, grease proofing and acid and alkali-resistance.

Description

A kind of preparation method of PFPE oil-based magnetic fluids material
Technical field
The present invention relates to a kind of magnetic fluid material and preparation method thereof, particularly relate to one and be applicable to dynamic vacuum sealing, harsh super quiet, hot environment and waterproof, grease proofing PFPE oil-based magnetic fluids material and preparation method thereof can be met, belong to material and preparing technical field thereof.
Background technology
Magnetic fluid is a kind of functional material invented by NASA middle 1960s, primarily of magnetic nano-particle, surfactant and liquid phase carrier three part composition.Nano particle Absorbable organic halogens is present in liquid phase carrier can not there is reunion and precipitation.Because it has superparamagnetic characteristic, therefore can respond fast under additional magnetic fields.Magnetic fluid can be applicable to industrial various aspects as vacuum seal, damping, lubrication etc.
As liquid phase carrier, PFPE has that steam forces down, chemical inertness, heat-resisting, the characteristic such as not fire, therefore greatly widened the range of application of magnetic fluid.This material has good application prospect in the field of sealing technology of ultra-clean ultra-high vacuum environment.
Summary of the invention
The object of the invention is to for deficiency of the prior art, the method of transition is utilized to make magnetic transfer of granules in carrier fluid, and introduce second surface activating agent and carry out aid dispersion, a kind of waterproof, grease proofing, acidproof PFPE oil-based magnetic fluids material and preparation method thereof are provided.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize:
A kind of preparation method of PFPE oil-based magnetic fluids material, utilize in situ Precipitation synthesis of nano magnetic particles of ferroferric oxide, while synthesis, utilize fluorine ether surfactant to modify as first surface activating agent, then with water and alcohol alternately cleaning, the magnetic particle obtained can be dispersed in transition liquid, finally utilize transition liquid aid dispersion surfactant, carrier fluid and magnetic particle to be dissolved each other, in the process of heating, remove transition liquid obtain the good PFPE oil-based magnetic fluids of dispersion effect;
Described first surface activating agent, fluorine ether surfactant structurefor: C 3f 7o [CF (CF 3) CF 2o] ncF (CF 3) CR
Wherein, n=3 ~ 50, R=OOH, SO 3m, PO (OH) 2;
The structure of described transition liquid is:
（1）CF 3(CF 2) mO(CH 2) nCH 3
Wherein, m=3-10, n=0-3
（2）CF 3(CF 2) mCF 2R
Wherein, m=1-10, R=CF 3, CH 2f, CCl 2f
The boiling point of transition liquid is lower than 150 DEG C;
The structure of described aid dispersion surfactant is:
(1) fluorine ether carboxylic acid and amino acid condensation reaction are formed
CF 3CF 2CF 2O[CF(CF 3)CF 2O] nCF(CF 3)COONHC(COOH)R
Wherein, n=3-50, R are the hydrocarbon chain structure in amino acid
(2) fluorine ether virtue acid amides
CF 3CF 2CF 2O[CF(CF 3)CF 2O] nCF（CF 3）COONHAr
Wherein, n=3-50, Ar are benzene ring structure;
Described carrier fluid structurefor:
（1）CF 3CF 2CF 2O[CF(CF 3)CF 2O] nC 2F 5
Wherein, n=10-50
A series of branch polymers that hexafluoropropylene (HFP) oxide is formed by being polymerized under CsF catalysis
（2）CF 3O(C 3F 6O) p(CF 2O) qCF 3。
Wherein, p=10-50, q=1-10
It is the polymer under the action of uv light hexafluoropropylene formed by photooxidation
（3）CF 3O(C 2F 4O) m(CF 2O) nCF3
Wherein, m=10-50, n=1-10
It is the straight chain polymer that tetrafluoroethene (TFE) is formed by photooxidation under the action of uv light
（4）C 3F 7O(CF 2CF 2CF 2O) nC 2F 5
Wherein, n=10-50
It is polymer product first directly fluoridized by polymerization by tetrafluoro oxetanes again and obtains.
Separately, the particle diameter of described nanometer Fe 3 O 4 magnetic particle is 10-15 nanometer.
Separately have, the heating-up temperature of described heating process is 150-180 DEG C.
Again, the mass ratio of described fluorine ether surfactant, aid dispersion surfactant and nanometer Fe 3 O 4 magnetic particle is 0.4 ~ 0.5:0.2 ~ 0.3:1.
Meanwhile, the mass ratio of described first surface activating agent, aid dispersion surfactant and nanometer Fe 3 O 4 magnetic particle is 0.45:0.25:1.
Compared with prior art, tool of the present invention has the following advantages:
1) the magnetic particle prepared of the present invention is through first surface activating agent modified, is not easy aging;
2) the transition liquid that the present invention uses can dissolve each other with the perfection of first surface active agent structures, in other words, described transition liquid both can dissolve each other with the magnetic-particle modified and also can dissolve each other with carrier fluid, use transition liquid magnetic particle and cosurfactant, carrier fluid in heating process to dissolve each other, dispersion effect heats than directly;
3) transition liquid is small molecule structure, boiling point lower than 150 DEG C so that remove in later stage heating process;
4) the aid dispersion surfactant of different structure is adopted to improve dispersion effect further.
Embodiment
Below in conjunction with specific embodiment, the present invention is elaborated.
embodiment 1
By divalent iron salt FeCl 2with trivalent iron salt FeCl 3by the molar ratio of 1:2, the alcohol emulsion prepared by 12g first surface activating agent (wherein R=OOH) is added under reaction temperature is 80 DEG C of conditions, then precipitation reagent ammoniacal liquor 100mL is added, salt acid for adjusting pH to 4 is added after reaction 1h, after distilled water and alcohol alternately clean, under magnetic fields, remove supernatant liquid, add 50mL transition liquid C 5h 2f 10, magnetic particle is dissolved in transition liquid, then removes the impurity such as unnecessary water under magnetic fields, and the liquid that takes a morsel records the content of magnetic particle, finally adds the carrier fluid CF of 20g 3cF 2cF 2o [CF (CF 3) CF 2o] 10c 2f 5with aid dispersion surfactant CF 3cF 2cF 2o [CF (CF 3) CF 2o] 3cF (CF 3) COONHC (COOH) C 3h 7
, obtained PFPE oil-based magnetic fluids after adding heat partition through 150 DEG C.
embodiment 2
By divalent iron salt FeCl 2with trivalent iron salt FeCl 3by the molar ratio of 1:2, add under reaction temperature is 80 DEG C of conditions by 12g first surface activating agent (wherein R=SO 3m) the alcohol emulsion prepared, then adds precipitation reagent ammoniacal liquor 100mL, adds salt acid for adjusting pH to 4 after reaction 1h, removes supernatant liquid, add 50mL transition liquid C after distilled water and alcohol alternately clean under magnetic fields 4f 9oC 2h 5, magnetic particle is dissolved in transition liquid, then removes the impurity such as unnecessary water under magnetic fields, and the liquid that takes a morsel records the content of magnetic particle, finally adds 20g carrier fluid CF 3o (C 3f 6o) 50(CF 2o) 10cF 3with aid dispersion surfactant CF 3cF 2cF 2o [CF (CF 3) CF 2o] ncF (CF 3) COONHC 6h 6, obtained PFPE oil-based magnetic fluids after adding heat partition through 180 DEG C.
embodiment 3
By divalent iron salt FeCl 2with trivalent iron salt FeCl 3by the molar ratio of 1:2, add under reaction temperature is 80 DEG C of conditions by 12g first surface activating agent (wherein R=PO (OH) 2) the alcohol emulsion prepared, then add precipitation reagent ammoniacal liquor 100mL, after reaction 1h, add salt acid for adjusting pH to 4, after distilled water and alcohol alternately cleaning, under magnetic fields, remove supernatant liquid, add suitable transition liquid C 13f 26cl 2, magnetic particle is dissolved in transition liquid, then removes the impurity such as unnecessary water under magnetic fields, and the liquid that takes a morsel records the content of magnetic particle, finally adds 20g carrier fluid C 3f 7o (CF 2cF 2cF 2o) 50c 2f 5with aid dispersion surfactant CF 3cF 2cF 2o [CF (CF 3) CF 2o] 50cF (CF 3) COONHC (COOH) C 8h 17, obtained PFPE oil-based magnetic fluids after adding heat partition through 150 DEG C.
The present invention can summarize with the concrete form without prejudice to spirit of the present invention or principal character; above-mentioned embodiment is only in order to illustrate technical scheme of the present invention but not to limit design of the present invention and protection range; those of ordinary skill of the present invention is modified to technical scheme of the present invention or equivalent replacement; and not departing from aim and the scope of technical scheme, it all should be encompassed in right of the present invention.

Claims (5)

1. the preparation method of a PFPE oil-based magnetic fluids material, it is characterized in that: utilize in situ Precipitation synthesis of nano magnetic particles of ferroferric oxide, while synthesis, utilize fluorine ether surfactant to modify as first surface activating agent, then with water and alcohol alternately cleaning, the magnetic particle obtained can be dispersed in transition liquid, finally utilize transition liquid aid dispersion surfactant, carrier fluid and magnetic particle to be dissolved each other, in the process of heating, remove transition liquid obtain the good PFPE oil-based magnetic fluids of dispersion effect; Described first surface activating agent, fluorine ether surfactant structurefor: C 3f 7o [CF (CF 3) CF 2o] ncF (CF 3) CR
Wherein, n=3 ~ 50, R=OOH, SO 3m, PO (OH) 2;
The structure of described transition liquid is:
（1）CF 3(CF 2) mO(CH 2) nCH 3
Wherein, m=3-10, n=0-3
（2）CF 3(CF 2) mCF 2R
Wherein, m=1-10, R=CF 3, CH 2f, CCl 2f
The boiling point of transition liquid is lower than 150 DEG C;
The structure of described aid dispersion surfactant is:
(1) fluorine ether carboxylic acid and amino acid condensation reaction are formed
CF 3CF 2CF 2O[CF(CF 3)CF 2O] nCF(CF 3)COONHC(COOH)R
Wherein, n=3-50, R are the hydrocarbon chain structure in amino acid
Fluorine ether virtue acid amides
CF 3CF 2CF 2O[CF(CF 3)CF 2O] nCF（CF 3）COONHAr
Wherein, n=3-50, Ar are benzene ring structure;
Described carrier fluid structurefor:
（1）CF 3CF 2CF 2O[CF(CF 3)CF 2O] nC 2F 5
Wherein, n=10-50
A series of branch polymers that hexafluoropropylene (HFP) oxide is formed by being polymerized under CsF catalysis
（2）CF 3O(C 3F 6O) p(CF 2O) qCF 3
Wherein, p=10-50, q=1-10
It is the polymer under the action of uv light hexafluoropropylene formed by photooxidation
（3）CF 3O(C 2F 4O) m(CF 2O) nCF3
Wherein, m=10-50, n=1-10
It is the straight chain polymer that tetrafluoroethene (TFE) is formed by photooxidation under the action of uv light
（4）C 3F 7O(CF 2CF 2CF 2O) nC 2F 5
Wherein, n=10-50
It is polymer product first directly fluoridized by polymerization by tetrafluoro oxetanes again and obtains.
2. the preparation method of a kind of PFPE oil-based magnetic fluids material according to claim 1, is characterized in that: the particle diameter of described nanometer Fe 3 O 4 magnetic particle is 10-15 nanometer.
3. the preparation method of a kind of PFPE oil-based magnetic fluids material according to claim 1, is characterized in that: the heating-up temperature of described heating process is 150-180 DEG C.
4. the preparation method of a kind of PFPE oil-based magnetic fluids material according to claim 1, is characterized in that: the mass ratio of described fluorine ether surfactant, aid dispersion surfactant and nanometer Fe 3 O 4 magnetic particle is 0.4 ~ 0.5:0.2 ~ 0.3:1.
5. the preparation method of a kind of PFPE oil-based magnetic fluids material according to claim 1, is characterized in that: the mass ratio of described first surface activating agent, aid dispersion surfactant and nanometer Fe 3 O 4 magnetic particle is 0.45:0.25:1.
CN201510729740.3A 2015-11-02 2015-11-02 A kind of preparation method of PFPE oil-based magnetic fluids material Pending CN105225786A (en)

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Citations (3)

* 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
CN103680799A (en) * 2013-12-17 2014-03-26 北京交通大学 Perfluor polyether oil-based magnetic liquid

Patent Citations (3)

* 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
CN103680799A (en) * 2013-12-17 2014-03-26 北京交通大学 Perfluor polyether oil-based magnetic liquid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王凡: "氟碳化合物基磁性液体制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

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Application publication date: 20160106