CN106298146B - A kind of new method for improving FeCoB/FeB magnetic liquid stability - Google Patents
A kind of new method for improving FeCoB/FeB magnetic liquid stability Download PDFInfo
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- CN106298146B CN106298146B CN201610945052.5A CN201610945052A CN106298146B CN 106298146 B CN106298146 B CN 106298146B CN 201610945052 A CN201610945052 A CN 201610945052A CN 106298146 B CN106298146 B CN 106298146B
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- 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
- H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
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Abstract
The present invention provides a kind of new method for preparing FeCoB/FeB magnetic liquids.By FeCl2·4H2The aqueous solution and/or CoCl of O2·6H2The aqueous solution of O is uniformly mixed with the mixed liquor of n-hexane, span80 and OP 10, obtains FeCl2Microemulsion and/or CoCl2Microemulsion；By NaBH4Aqueous solution, be uniformly mixed with the mixed liquor of n-hexane, span80 and OP 10, obtain NaBH4Microemulsion；By above-mentioned FeCl2Microemulsion and/or CoCl2Microemulsion and NaBH4Microemulsion is uniformly mixed, normal-temperature reaction, removes precipitation to get FeCoB magnetic liquids.Step is simple and convenient to operate, is highly practical.
Description
Technical field
The invention belongs to magnetic liquid preparation field, more particularly to a kind of raising FeCoB/FeB magnetic liquid stability
New method.
Background technology
Magnetic liquid is as a kind of functional material for having both magnetic performance and liquid fluidity, in sealing, lubrication, medicine target
It has a wide range of applications to treatment etc..The quality of magnetic liquid stability directly affects its service life.It is current to improve
The conventional method of magnetic liquid stability is that surface modification is carried out to magnetic-particle, and principle is to add in surfactant, surface
The both ends of activating agent generate chemical bond with carrier fluid and magnetic-particle surface respectively, do not occur so that particle is dispersed in carrier fluid
Sedimentation and reunite [Fang, F.F.；Hyoung,J.Sequential coating of magnetic carbonyliron
particles with polystyrene and multiwalled carbon nanotubes and its effect on
theirmagnetorheology.ACS Appl.Mater.Interf.2010,2,54–60.].This method is to Fe3O4,
ZnFe2O4,CoFe2O4Wait magnetic-particles that there is good effect.But for the good particle of part magnetic performance, such as
The soft magnetic granules such as FeCoB, FeB, this method are extremely difficult to preferably improve the effect of stability, the reason is that this particle
Surface can not generate chemically combined functional group with surfactant.This seriously inhibits using FeCoB, FeB etc. as magnetism
The preparation of the magnetic liquid of particle.Therefore, a kind of method of the new raising stability being also adapted to such magnetic-particle is found
With critically important practical significance.
《Novel magnetic materials --- the preparation of Co-B magnetic fluids》It discloses a kind of sodium borohydride reduction and prepares Co-B magnetic
The method of fluid, but this method preparation process is cumbersome, is related to the separation of magnetic-particle, and separation process can produce beads magnetic
It is raw to influence.
《Microemulsion method prepares ferrite magnetic material progress》Using TritonX-100/ n-hexyl alcohols/n-hexane/water as
Reaction medium has synthesized spinel-type CoFe of the particle size range in 15~50nm using double microemulsion methods2O4Magnetic-particle.But its
Can not still meet prepare particle smaller, particle size evenly, dispersiveness preferably high stability magnetic liquid requirement.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of method of new raising magnetic liquid stability.It obtains
FeCoB magnetic liquids/FeB magnetic liquids stability is high, and particle surface is not modified, and solves FeCoB/FeB
Particle may not apply to the preparation problem of magnetic liquid because of that cannot be surface modified.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method for improving FeB magnetic liquid stability, including：
By FeCl2·4H2The aqueous solution of O is uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtains FeCl2It is micro-
Lotion；
By NaBH4Aqueous solution, be uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtain NaBH4Microemulsion；
By above-mentioned FeCl2Microemulsion and NaBH4Microemulsion is uniformly mixed, normal-temperature reaction, and it is magnetic to get FeB to remove precipitation
Liquid.
Present system has studied dispersed rule of the FeCoB/FeB particles in microemulsion environment, finds：Using
Span80 and OP-10 are compounded in particular range, can effectively sum it up Fe, B or Co ion, obtained particle size about 10nm,
In good monodispersity, and in this case, magnetic nanoparticle can be limited in the water phase of microemulsion system and
Separation sedimentation is not susceptible to, the magnetic liquid of acquisition has preferably stability and magnetization property.
Span80 refers in the present invention：Sorbester p17.
OP-10 refers in the present invention：Polyoxethylene octylphenyl phenol ether -10.
Preferably, the FeCl2Microemulsion and NaBH4In microemulsion, FeCl2With NaBH4Molar ratio be 1：3~3.2.
Preferably, the FeCl2·4H2The molar concentration of the aqueous solution of O is less than 2mol/L.
High spot reviews of the present invention influence of the microemulsion method preparation process to the stability of the magnetic liquid of preparation.Study table
It is bright：The amount and Fe of surfactant2+Concentration have a great impact to FeCoB/FeB magnetic liquid stability, work as Fe2+It is dense
When spending big, surfactant excessive or very few, the magnetic liquid stability of preparation is all poor.This is because in such case
The particle of lower preparation is larger, and the microemulsion system being formed simultaneously is unstable.
Preferably, the n-hexane, span80, OP-10, FeCl2·4H2In the aqueous solution of O the volume ratio of solvent for 28~
30：6.5~7.5：6.5~7.5：9~11.When the sum of volume parts of span80 and OP-10 are more than 15, the FeCoB/ of synthesis
FeB magnetic liquids dispersiveness declines, particle is easily reunited；When the sum of volume parts of span80 and OP-10 are less than 13, synthesis
FeCoB/FeB magnetic liquids stability declines, is layered.
The present invention also provides it is a kind of improve FeCoB magnetic liquid stability method, including：
By FeCl2·4H2The aqueous solution of O is uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtains FeCl2It is micro-
Lotion；
By CoCl2·6H2The aqueous solution of O is uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtains CoCl2It is micro-
Lotion；
By NaBH4Aqueous solution, be uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtain NaBH4Microemulsion；
By above-mentioned FeCl2Microemulsion, CoCl2Microemulsion and NaBH4Microemulsion is uniformly mixed, normal-temperature reaction, and it is heavy to remove
It forms sediment to get FeCoB magnetic liquids.
Preferably, the FeCl2Microemulsion, CoCl2Microemulsion and NaBH4In microemulsion, FeCl2、CoCl2、NaBH4Rub
You are than being 1：1：6~6.4.
Preferably, the FeCl2·4H2The molar concentration of the aqueous solution of O is less than 1mol/L.
Preferably, the n-hexane, span80, OP-10, FeCl2·4H2In the aqueous solution of O the volume ratio of solvent for 28~
30：6.5~7.5：6.5~7.5：9~11.
In the present invention, for the ternary system of water, n-hexane, span80 and OP-10, the addition of alcohol is simultaneously not yet in effect
Ground improves interfacial film and obtains mobility, therefore, due to cost considerations, alcoholic solution is not added in the present invention.
The present invention also provides it is a kind of improve CoB magnetic liquid stability method, including：
By CoCl2·6H2The aqueous solution of O is uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtains CoCl2It is micro-
Lotion；
By NaBH4Aqueous solution, be uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtain NaBH4Microemulsion；
By above-mentioned CoCl2Microemulsion and NaBH4Microemulsion is uniformly mixed, normal-temperature reaction, and it is magnetic to get CoB to remove precipitation
Liquid.
FeB magnetic liquids, FeCoB magnetic liquids, CoB magnetic liquids the present invention also provides above method preparation is close
Application in envelope, lubrication, drug targeting treatment.
It is as follows including step the present invention also provides a kind of new process of preferably FeCoB/FeB magnetic liquids：
(1)FeCl2、CoCl2Microemulsion/FeCl2The preparation of microemulsion：By (FeCl2·4H2O、CoCl2·6H2O)/
FeCl2·4H2O is added among a certain amount of distilled water, and stirring is added dropwise to just to being completely dissolved, then by dissolved solution
Among the mixed liquor of hexane and span80, OP-10, it is sufficiently stirred, obtains FeCl2、CoCl2Microemulsion/FeCl2Microemulsion.
(2)NaBH4The preparation of microemulsion：By a certain amount of NaBH4It is added among distilled water and stirs to being completely dissolved,
Dissolved solution is added dropwise among the mixed liquor of n-hexane and span80, OP-10 again, low speed is sufficiently stirred, and is obtained
NaBH4Microemulsion.
(3) preparation of FeCoB magnetic liquids/FeB magnetic liquids：The NaBH that step (2) is obtained4Microemulsion is added dropwise
The FeCl obtained to step (1)2、CoCl2Microemulsion/FeCl2In microemulsion, when stirring 0.5-1 is small, partly precipitated is removed, is obtained
FeCoB magnetic liquids/FeB magnetic liquids.
In step (1), (2), n-hexane, span80, OP-10, water addition volume ratio be n-hexane：span80：
OP-10：Water is 28~30：6.5~7.5：6.5~7.5：9~11.
In step (1), when preparing FeCoB magnetic liquids, FeCl2·4H2The molar concentration of O should be controlled within 1mol/L；
When preparing FeB magnetic liquids, FeCl2·4H2The molar concentration of O should be controlled within 2mol/L.Excessively high concentration can make stability
Decline.
In step (1), when preparing FeCoB magnetic liquids, FeCl2·4H2O、CoCl2·6H2The adding proportion of O is mole
Than 1:1.
In step (2), NaBH4Amount of substance should be FeCl in step (1)2·4H26 times of O (prepare FeCoB magnetic liquids
When) or 3 times (when preparing FeB magnetic liquids).NaBH4Microemulsion concentration is advisable with approaching its saturated concentration.
In step (3), NaBH4The rate of addition of microemulsion using system after being added dropwise react when be not in a large amount of bubbles as
It is accurate.
In step (1-3), all operations step should be completed at 20 DEG C.
In step (1-3), all stirrings being related to are low-speed machinery stirring.
Beneficial effects of the present invention
(1) the FeCoB magnetic liquids/FeB magnetic liquids stability that the present invention obtains are high, and not to particle surface into
Row modification, solves the problems, such as that FeCoB/FeB particles may not apply to the preparation of magnetic liquid because of that cannot be surface modified.
The raising of stability is (as shown in Figure 4) realized by following mechanism in the present invention：Using span80, OP-10 as emulsifier, just
Water/n-hexane microemulsion is prepared for oil phase in hexane, in water phase of the nano magnetic particle in magnetic liquid in microemulsion
Reaction generation.The interfacial tension of water phase oil phase makes nano magnetic particle be limited in water phase and cannot pass through interface in microemulsion,
So as to avoid the mutual reunion and sedimentation between particle.The surface modification of particle is not related in the process.
(2) preparation method of the present invention is simple, detection efficiency is high, highly practical, easy to spread.
Description of the drawings
Fig. 1 is embodiment 1, the VSM figures of 2 gained magnetic liquids；
Fig. 2 is embodiment 1, the particle SEM figures of 2 gained magnetic liquids；
Fig. 3 is embodiment 1, the magnetic weightening graph of 2 gained magnetic liquids.
Fig. 4 is the mechanism figure of magnetic liquid.
Wherein, example 1, example 2 correspond to embodiment 1, embodiment 2 respectively.
Specific embodiment
Feature of present invention and other correlated characteristics are described in further detail by the following examples, in order to the same industry
The understanding of technical staff：
Embodiment 1:
Raw material have：FeCl2·4H2O、CoCl2·6H2O、NaBH4, n-hexane, span80, OP-10, distilled water.It is all
Reagent is that analysis is pure.
A kind of new process for preparing high-stability Fc CoB magnetic liquids, it is as follows including step：
(1)FeCl2、CoCl2The preparation of microemulsion：1.0g FeCl are weighed respectively2·4H2O、1.2g CoCl2·6H2O is simultaneously
It is added among 7ml distilled water, stirring at low speed is added dropwise to n-hexane (22ml) to being completely dissolved, then by dissolved solution
With span80 (4.7ml), OP-10 (4.7ml) mixed liquor among, be sufficiently stirred, obtain FeCl2、CoCl2Microemulsion.
(2)NaBH4The preparation of microemulsion：Weigh 1.2g NaBH4It is added in 2ml distilled water and stirs to being completely dissolved,
Dissolved solution is added dropwise to n-hexane (6ml) again and span80 (1.3ml), the mixed liquor of OP-10 (1.3ml) are worked as
In, low speed is sufficiently stirred, and obtains NaBH4Microemulsion.
(3) preparation of FeCoB magnetic liquids：The NaBH that step (2) is obtained4Microemulsion is slowly added into step dropwise
(1) FeCl obtained2、CoCl2In microemulsion, when mechanical stirring at low speed 1 is small, partly precipitated is removed, obtains FeCoB magnetic liquids.
Embodiment 2:
Raw material have：FeCl2·4H2O、NaBH4, n-hexane, span80, OP-10, distilled water.All reagents are analysis
It is pure.
A kind of new process for preparing high-stability Fc B magnetic liquids, it is as follows including step：
(1)FeCl2The preparation of microemulsion：Weigh 2.7g FeCl2·4H2O is added among 7ml distilled water, stirring at low speed
N-hexane (22ml) and span80 (4.7ml), OP-10 (4.7ml) are added dropwise to being completely dissolved, then by dissolved solution
Mixed liquor among, be sufficiently stirred, obtain FeCl2Microemulsion.
(2)NaBH4The preparation of microemulsion：Weigh 1.59g NaBH4It is added in 2ml distilled water and stirs to being completely dissolved,
Dissolved solution is added dropwise to n-hexane (6ml) again and span80 (1.3ml), the mixed liquor of OP-10 (1.3ml) are worked as
In, low speed is sufficiently stirred, and obtains NaBH4Microemulsion.
(3) preparation of FeCoB magnetic liquids：The NaBH that step (2) is obtained4Microemulsion is slowly added into step dropwise
(1) FeCl obtained2In microemulsion, when mechanical stirring at low speed 1 is small, partly precipitated is removed, obtains FeB magnetic liquids.
Embodiment 3:
Raw material have：FeCl2·4H2O、CoCl2·6H2O、NaBH4, n-hexane, span80, OP-10, distilled water.It is all
Reagent is that analysis is pure.
A kind of new process for preparing high-stability Fc CoB magnetic liquids, it is as follows including step：
(1)FeCl2、CoCl2The preparation of microemulsion：1.0g FeCl are weighed respectively2·4H2O、1.2g CoCl2·6H2O is simultaneously
It is added among 9ml distilled water, stirring at low speed is added dropwise to n-hexane (24ml) to being completely dissolved, then by dissolved solution
With span80 (5.1ml), OP-10 (5.1ml) mixed liquor among, be sufficiently stirred, obtain FeCl2、CoCl2Microemulsion.
(2)NaBH4The preparation of microemulsion：Weigh 1.2g NaBH4It is added in 2ml distilled water and stirs to being completely dissolved,
Dissolved solution is added dropwise to n-hexane (7ml) again and span80 (1.5ml), the mixed liquor of OP-10 (1.5ml) are worked as
In, low speed is sufficiently stirred, and obtains NaBH4Microemulsion.
(3) preparation of FeCoB magnetic liquids：The NaBH that step (2) is obtained4Microemulsion is slowly added into step dropwise
(1) FeCl obtained2、CoCl2In microemulsion, when mechanical stirring at low speed 1 is small, partly precipitated is removed, obtains FeCoB magnetic liquids.
Embodiment 4:
Raw material have：FeCl2·4H2O、NaBH4, n-hexane, span80, OP-10, distilled water.All reagents are analysis
It is pure.
A kind of new process for preparing high-stability Fc B magnetic liquids, it is as follows including step：
(1)FeCl2The preparation of microemulsion：Weigh 2.7g FeCl2·4H2O is added among 7.6ml distilled water, and low speed stirs
It mixes to being completely dissolved, then dissolved solution is added dropwise to n-hexane (23ml) and span80 (4.9ml), OP-10
It among the mixed liquor of (4.9ml), is sufficiently stirred, obtains FeCl2Microemulsion.
(2)NaBH4The preparation of microemulsion：Weigh 1.59g NaBH4It is added in 2ml distilled water and stirs to being completely dissolved,
Dissolved solution is added dropwise to n-hexane (6.7ml) again and span80 (1.4ml), the mixed liquor of OP-10 (1.4ml) are worked as
In, low speed is sufficiently stirred, and obtains NaBH4Microemulsion.
(3) preparation of FeCoB magnetic liquids：The NaBH that step (2) is obtained4Microemulsion is slowly added into step dropwise
(1) FeCl obtained2In microemulsion, when mechanical stirring at low speed 1 is small, partly precipitated is removed, obtains FeB magnetic liquids.
Comparative example：
By attached drawing 1 it can be seen that the magnetic liquid prepared has good superparamagnetism, while compare it can be found that two
The species of particle is different with the additive amount of magnetic-particle in example, and the saturation magnetization of magnetic liquid obtained is different, changes speech
It, the saturation magnetization for the magnetic liquid that such method obtains can be adjusted by changing additive amount and the species of magnetic-particle
Section；It can be seen that the nanoparticle size about 10nm prepared by attached drawing 2 and there is dispersiveness well, this is to magnetic liquid
Stability has important influence；By attached drawing 3 it can be seen that two kinds of magnetic liquids have good stability, even if larger additional
It is not easy to precipitate under magnetic field.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, this hair is not limited to
It is bright, although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, still
It can modify to the technical solution recorded in previous embodiment or equivalent substitution is carried out to which part.It is all in this hair
Within bright spirit and principle, any modifications, equivalent replacements and improvements are made should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
The various modifications or changes that can be made are made the creative labor still within protection scope of the present invention.
Claims (4)
- A kind of 1. method for improving FeB magnetic liquid stability, which is characterized in that including：By FeCl2•4H2The aqueous solution of O, with The mixed liquor of n-hexane, span80 and OP-10 is uniformly mixed, and obtains FeCl2Microemulsion；By NaBH4Aqueous solution, with n-hexane, The mixed liquor of span80 and OP-10 is uniformly mixed, and obtains NaBH4Microemulsion；By FeCl2Microemulsion and NaBH4Microemulsion mixing is equal Even, normal-temperature reaction removes precipitation to get FeB magnetic liquids；The FeCl2Microemulsion and NaBH4In microemulsion, FeCl2With NaBH4Molar ratio be 1：3~3.2；The FeCl2•4H2The molar concentration of the aqueous solution of O is less than 2mol/L；The n-hexane, span80, OP-10, FeCl2•4H2The volume ratio of solvent is 28 ~ 30 in the aqueous solution of O：6.5~7.5： 6.5~7.5：9~11.
- A kind of 2. method for improving FeCoB magnetic liquid stability, which is characterized in that including：By FeCl2•4H2The aqueous solution of O, It is uniformly mixed with the mixed liquor of n-hexane, span80 and OP-10, obtains FeCl2Microemulsion；By CoCl2•6H2The aqueous solution of O, and just The mixed liquor of hexane, span80 and OP-10 is uniformly mixed, and obtains CoCl2Microemulsion；By NaBH4Aqueous solution, with n-hexane, The mixed liquor of span80 and OP-10 is uniformly mixed, and obtains NaBH4Microemulsion；By FeCl2Microemulsion, CoCl2Microemulsion and NaBH4It is micro- Lotion is uniformly mixed, normal-temperature reaction, removes precipitation to get FeCoB magnetic liquids；The FeCl2Microemulsion, CoCl2Microemulsion and NaBH4In microemulsion, FeCl2、CoCl2、NaBH4Molar ratio be 1：1：6 ~6.4；The FeCl2•4H2The molar concentration of the aqueous solution of O is less than 1mol/L；The n-hexane, span80, OP-10, FeCl2•4H2The volume ratio of solvent is 28 ~ 30 in the aqueous solution of O：6.5~7.5： 6.5~7.5：9~11.
- A kind of 3. method for improving CoB magnetic liquid stability, which is characterized in that including：By CoCl2•6H2The aqueous solution of O, with The mixed liquor of n-hexane, span80 and OP-10 is uniformly mixed, and obtains CoCl2Microemulsion；By NaBH4Aqueous solution, with n-hexane, The mixed liquor of span80 and OP-10 is uniformly mixed, and obtains NaBH4Microemulsion；By CoCl2Microemulsion and NaBH4Microemulsion mixing is equal Even, normal-temperature reaction removes precipitation to get CoB magnetic liquids.
- 4. FeCoB magnetism liquid prepared by FeB magnetic liquids prepared by claim 1 the method, claim 2 the method The application of CoB magnetic liquids prepared by the method described in body, claim 3 in sealing, lubrication, drug targeting treatment.
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