CN103531323A - Preparation method for magnetic liquid without surfactants - Google Patents
Preparation method for magnetic liquid without surfactants Download PDFInfo
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- CN103531323A CN103531323A CN201310537542.8A CN201310537542A CN103531323A CN 103531323 A CN103531323 A CN 103531323A CN 201310537542 A CN201310537542 A CN 201310537542A CN 103531323 A CN103531323 A CN 103531323A
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Abstract
The invention belongs to the technical field of materials`, in particular to a preparation method for magnetic liquid without surfactants, and aims at providing the preparation method for magnetic liquid without surfactants. According to the technical scheme, the preparation method for magnetic liquid without surfactants comprises the steps of preparing iron oxide nanoparticle dispersion phases; preparing dispersion medium carrier liquid; compounding magnetic liquid. The preparation method can be used for preparation of magnetic liquid.
Description
Technical field
The invention belongs to material technology field, be specifically related to the preparation method of surfactant-free magnetic liquid.
Background technology
Magnetic liquid is that magnetic nanometer particles (adopting ferric oxide nano particulate) is scattered in the soliquid forming in non magnetic carrier fluid more as Magnetic Phase, its physical property---as optical property, viscosity characteristics etc., the liquid functional material that can be regulated and controled by external magnetic field, the magnetic after effect having without solid magnetic material.For avoiding the sedimentation separation that particulate produces due to Action of Gravity Field in carrier fluid, the particle diameter of the magnetic nanometer particles in magnetic liquid is limited in 10nm left and right.For avoiding magnetic nanometer particles because the particulate of van der waals force and magnetostatic coupling generation is reunited, magnetic particle need wrap up surfactant conventionally, and the space bit producing by surfactant long-chain molecule is made every effort to overcome the reunion trend that takes particulate.This magnetic liquid is referred to as surfactant type magnetic liquid.The response speed that the field of this magnetic liquid causes effect will be subject to the impact of surfactant, and the fluid mechanics particle diameter of its particulate is greater than its intrinsic physics particle diameter.In addition, dispersible particulate makes its microparticle surfaces absorption hydrogen ion and forms charged corpuscle in acid base fluid, and the electrostatic repulsion that relies on like charges to produce overcomes the reunion between particulate.This magnetic liquid is referred to as ionic or two galvanic couple stratotype magnetic liquid.In ionic ferrofluid, fluid mechanics particle diameter is identical with physics particle diameter.Therefore the ionic and the surface active formulation magnetic liquid that for the chemical composition magnetic nanometer particles identical with physics particle diameter, form, the former field causes response speed faster than the latter.For avoiding ferric oxide particles to be dissolved by acid, the ferric oxide particles in ionic ferrofluid need adopt ferric nitrate to process to form the protective layer of surperficial antiacid erosion conventionally, uses aqueous solution of nitric acid as decentralized medium carrier fluid.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of the magnetic liquid without surfactant.
Technical scheme of the present invention is the preparation method of surfactant-free magnetic liquid, comprises the steps:
The preparation of a, ferric oxide nano microparticulate phase: in alkaline medium, by chemical precipitation method, prepare alkali formula hydroxide iron-based presoma, clean to pH be 7～8, obtain presoma; In solution of ferrous chloride, presoma is processed, after cleaning, dewater, being dried, can be obtained ferric oxide nano particulate;
The preparation of b, decentralized medium carrier fluid: the mixed liquor of glycerine-water, as decentralized medium carrier fluid, adds nitric acid to regulate and control the concentration of acid decentralized medium;
Synthesizing of c, magnetic liquid: under stirring, the ferric oxide nano particulate as decentralized photo is mixed with the decentralized medium as carrier fluid, natural aging obtains the magnetic liquid of stable chemical nature after 10 days; The ratio of decentralized photo and decentralized medium is represented by decentralized photo volume fraction:
Wherein, Φ v is 0.0001～0.025.
Preferably, Φ v is 0.02.
Wherein, the volume ratio of described Gan You ︰ water is 10～95 ︰ 90～5.
Most preferably, the volume ratio of described Gan You ︰ water is 60 ︰ 40.
Wherein, in solution of ferrous chloride, presoma is processed described in step a: using 0.5 molar concentration solution of ferrous chloride as treatment fluid, the volume ratio of presoma and treatment fluid is 1 ︰ 5, heat treated liquid is to boiling, then under agitation presoma is poured in treatment fluid, keep boiling within 30 minutes, to stop heating, be cooled to ferric oxide nano particulate and separate out gradually.
Wherein, the cleaning described in step a, dehydration refer to: with distilled water, clean ferric oxide nano particulate, then with acetone, dewater.
Wherein, the concentration of nitric acid in decentralized medium is
mol/L, Z in formula
bthe chemical valence of the acid ion in carrier fluid decentralized medium, ρ
sdensity g/cm for nanoparticle decentralized photo
3, M
wsmolecular weight for nanoparticle decentralized photo; Φ v decentralized photo volume fraction.
The present invention proposes without surfactant the ionic ferrofluid preparation method who is formed by iron oxide magnetic nano particulate.In the ionic ferrofluid preparation method who proposes in the present invention, iron oxide magnetic nano particle does not need to process and form antiacid erosion layer through ferric nitrate, the substitute is particulate and in preparation process, forms antiacid erosion superficial layer.The magnetic liquid of being prepared by this method, magnetic nanometer particles does not wherein have the surfactant parcel of long-chain, so that compare so that compare with common surface active formulation magnetic liquid the material not only consuming with common surface active formulation magnetic liquid less, simplified synthesis technique step, and there is faster field and cause response speed.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of magnetic nanometer particles.
Fig. 2 is the ratio magnetization curve of magnetic nanometer particles.Abscissa in figure is magnetic field intensity, and ordinate is specific magnetization.
The ratio magnetization curve of magnetic liquid in Fig. 3 embodiment 1.
The ratio magnetization curve of magnetic liquid in Fig. 4 embodiment 2.
The ratio magnetization curve of magnetic liquid in Fig. 5 embodiment 3.
Embodiment
The preparation method of surfactant-free magnetic liquid of the present invention comprises the steps:
The preparation of a, ferric oxide nano microparticulate phase: in alkaline medium, by chemical precipitation method, prepare alkali formula hydroxide iron-based presoma, clean to pH be 7～8, obtain presoma; In solution of ferrous chloride, presoma is processed, after cleaning, dewater, being dried, can be obtained ferric oxide nano particulate;
The preparation of b, decentralized medium carrier fluid: the mixed liquor of glycerine-water, as decentralized medium carrier fluid, adds nitric acid to regulate and control the concentration of acid decentralized medium;
Synthesizing of c, magnetic liquid: under stirring, the ferric oxide nano particulate as decentralized photo is mixed with the decentralized medium as carrier fluid, natural aging obtains the magnetic liquid of stable chemical nature after 10 days; The ratio of decentralized photo and decentralized medium is represented by decentralized photo volume fraction:
Wherein, Φ v is 0.0001～0.025.
Preferably, Φ v is 0.02.
Wherein, the volume ratio of described Gan You ︰ water is 10～95 ︰ 90～5.
Most preferably, the volume ratio of described Gan You ︰ water is 60 ︰ 40.
Wherein, in solution of ferrous chloride, presoma is processed described in step a: using 0.5 molar concentration solution of ferrous chloride as treatment fluid, the volume ratio of presoma and treatment fluid is 1 ︰ 5, heat treated liquid is to boiling, then under agitation presoma is poured in treatment fluid, keep boiling within 30 minutes, to stop heating, be cooled to ferric oxide nano particulate and separate out gradually.
Wherein, the cleaning described in step a, dehydration refer to: with distilled water, clean ferric oxide nano particulate, then with acetone, dewater.
Wherein, the concentration of nitric acid in decentralized medium is
mol/L, Z in formula
bthe chemical valence of the acid ion in carrier fluid decentralized medium, ρ
sdensity g/cm for nanoparticle decentralized photo
3, M
wsmolecular weight for nanoparticle decentralized photo; Φ v decentralized photo volume fraction.
In the present invention, if Φ v<0.0001, the field of magnetic liquid cause character very a little less than, lose the feature of magnetic functional material; If Φ is v>0.025, may there is precipitation in the particulate in magnetic liquid.Through research, finding, is the better performances of 0.02 magnetic liquid at Φ v.
In the present invention, inventor finds that by test of many times the volume ratio of Gan You ︰ water is 10～95 ︰ 90～5 o'clock, the better performances of resulting magnetic liquid.Especially, when the volume ratio of Gan You ︰ water is 60 ︰ 40, reach best.
Embodiment 1 adopts the inventive method to prepare magnetic liquid
The preparation of first step ferric oxide nano particulate
(1) presoma preparation
Take ferric trichloride and nickel nitrate as raw material, and the aqueous solution that the ratio that is 2 ︰ 1 with the mol ratio of nickel in iron is chosen both mixes.The sodium hydroxide solution of 0.7 molar concentration of 10 times of volumes is poured in ferric trichloride-nickel nitrate mixed liquor, be then heated to boiling, after seething with excitement 5 minutes, stop heating, naturally cool to room temperature.Presoma Precipitation gradually in cooling procedure.
With the aqueous solution of nitric acid of 0.01 molar concentration as cleaning fluid.By sediment and the volume ratio of cleaning fluid, be that 1 ︰ 5 mixes, fully stir by centrifuge separation, repeat this step 3 time.
(2) preparation of magnetic nanometer particles
Using 0.5 molar concentration solution of ferrous chloride as treatment fluid.According to the volume ratio of presoma and treatment fluid, be that 1:5 chooses appropriate treatment fluid, heat treated liquid, to boiling, is then under agitation poured presoma in treatment fluid into, keeps boiling within 30 minutes, to stop heating.Naturally cool to room temperature, in cooling procedure, nanoparticle is separated out gradually.
With distilled water washing and precipitating thing secondary, then with acetone dehydration three times.Sediment after dehydration is put into silica gel drier, obtains dry anhydrous magnetic nanometer particles powder after twenty four hours.
The transmission electron microscope of prepared magnetic nanometer particles resembles as shown in Figure 1, than magnetization curve as shown in Figure 2.
The preparation of second step decentralized medium
In the ratio of glycerine and water, be 10 ︰ 90 configuration decentralized medium carrier fluids.Preparation Φ
v=0.02 magnetic liquid, concentration of nitric acid is 4.46 * 10
-2mol/L.
The 3rd step magnetic liquid is synthetic
The ratio that is 2 ︰ 98 in the volume ratio of magnetic nanometer particles powder and carrier fluid is chosen nanoparticle powder and carrier fluid.Nanoparticle powder is scattered in to synthetic particulate volume fraction Φ in carrier fluid
vit is 0.02 magnetic liquid.
After standing 10 days, obtain magnetic liquid.
Synthesized magnetic liquid than magnetization curve as shown in Figure 3, is compared with the magnetization curve of the magnetic nanometer particles powder shown in Fig. 2, and both have similar shape as seen, the magnetization character of hence one can see that prepared magnetic liquid kept magnetic nanometer particles.Embodiment 2 adopts the inventive method to prepare magnetic liquid
The preparation of first step ferric oxide nano particulate
As embodiment 1.
The preparation of second step decentralized medium
In the ratio of glycerine and water, be 60 ︰ 40 preparation decentralized medium carrier fluids.Preparation Φ
v=0.02 magnetic liquid, concentration of nitric acid is 4.46 * 10-
2mol/L.
The 3rd step magnetic liquid is synthetic
The ratio that is 2 ︰ 98 in the volume ratio of magnetic nanometer particles powder and carrier fluid is chosen nano-powder and carrier fluid.Nanoparticle powder is scattered in to synthetic particulate volume fraction Φ in carrier fluid
vit is 0.02 magnetic liquid.
After standing 10 days, obtain magnetic liquid.
The ratio magnetization curve of synthesized magnetic liquid as shown in Figure 4.
The preparation of first step ferric oxide nano particulate
As embodiment 1.
The preparation of second step decentralized medium
In the ratio of glycerine and water, be 94 ︰ 6 preparation decentralized medium carrier fluids.Preparation Φ
v=0.02 magnetic liquid, concentration of nitric acid is 4.46 * 10
-2mol/L.
The 3rd step magnetic liquid is synthetic
The ratio that is 2 ︰ 98 in the volume ratio of magnetic nanometer particles powder and carrier fluid is chosen nano-powder and carrier fluid.Nanoparticle powder is scattered in to synthetic particulate volume fraction Φ in carrier fluid
vit is 0.02 magnetic liquid.
After standing 10 days, obtain magnetic liquid.
The ratio magnetization curve of synthesized magnetic liquid as shown in Figure 5.
Claims (8)
1. the preparation method of surfactant-free magnetic liquid, is characterized in that: comprise the steps:
The preparation of a, ferric oxide nano microparticulate phase: in alkaline medium, by chemical precipitation method, prepare alkali formula hydroxide iron-based presoma, clean to pH be 7～8, obtain presoma; In solution of ferrous chloride, presoma is processed, after cleaning, dewater, being dried, can be obtained ferric oxide nano particulate;
The preparation of b, decentralized medium carrier fluid: the mixed liquor of glycerine-water, as decentralized medium carrier fluid, adds nitric acid to regulate and control the concentration of acid decentralized medium;
Synthesizing of c, magnetic liquid: under stirring, the ferric oxide nano particulate as decentralized photo is mixed with the decentralized medium as carrier fluid, natural aging obtains the magnetic liquid of stable chemical nature after 10 days; The ratio of decentralized photo and decentralized medium is represented by decentralized photo volume fraction:
2. as the preparation method of claim 1 liquid, it is characterized in that: Φ v is 0.0001～0.025.
3. preparation method as claimed in claim 2, is characterized in that: Φ v is 0.02.
4. the preparation method as described in claim 1～3 any one, is characterized in that: the volume ratio of described Gan You ︰ water is 10～95 ︰ 90～5.
5. preparation method as claimed in claim 4, is characterized in that: the volume ratio of described Gan You ︰ water is 60 ︰ 40.
6. the preparation method as described in claim 1～5 any one, it is characterized in that: in solution of ferrous chloride, presoma is processed described in step a: using 0.5 molar concentration solution of ferrous chloride as treatment fluid, the volume ratio of presoma and treatment fluid is 1 ︰ 5, heat treated liquid is to boiling, then under agitation presoma is poured in treatment fluid, keep boiling within 30 minutes, to stop heating, be cooled to ferric oxide nano particulate and separate out gradually.
7. the preparation method as described in claim 1～6 any one, is characterized in that: the cleaning described in step a, dehydration refer to: with distilled water, clean ferric oxide nano particulate, then with acetone, dewater.
8. the preparation method as described in claim 1～7 any one, is characterized in that: the concentration of nitric acid in decentralized medium is
mol/L, Z in formula
bthe chemical valence of the acid ion in carrier fluid decentralized medium, ρ
sdensity g/cm for nanoparticle decentralized photo
3, M
wsmolecular weight for nanoparticle decentralized photo; Φ v decentralized photo volume fraction.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063502A (en) * | 2019-12-19 | 2020-04-24 | 华中科技大学 | Magnetic fluid with adjustable stability and preparation and recovery method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002075724A (en) * | 2000-08-30 | 2002-03-15 | Nok Corp | Method of manufacturing magnetic fluid |
| CN102910682A (en) * | 2012-09-29 | 2013-02-06 | 西南大学 | Preparation method of gamma-Fe2O3/ZnFe2O4 magnetic composite nano particle |
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- 2013-11-04 CN CN201310537542.8A patent/CN103531323A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002075724A (en) * | 2000-08-30 | 2002-03-15 | Nok Corp | Method of manufacturing magnetic fluid |
| CN102910682A (en) * | 2012-09-29 | 2013-02-06 | 西南大学 | Preparation method of gamma-Fe2O3/ZnFe2O4 magnetic composite nano particle |
Non-Patent Citations (3)
| Title |
|---|
| 傅俊: "一种二元离子型磁性液体的制备及磁化、磁光性质的研究", 《中国优秀硕士学位论文全文数据库基础科学辑》 * |
| 傅俊: "水-甘油基离子型磁性液体的合成及其磁化性质", 《西南大学学报(自然科学版)》 * |
| 赵正莹: "由Ni2O3/Fe2O3复合纳米微粒构成的离子型磁性液体的磁化性质研究", 《西南大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063502A (en) * | 2019-12-19 | 2020-04-24 | 华中科技大学 | Magnetic fluid with adjustable stability and preparation and recovery method thereof |
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Application publication date: 20140122 |