CN103632798B - A kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid - Google Patents
A kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid Download PDFInfo
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- CN103632798B CN103632798B CN201310636021.8A CN201310636021A CN103632798B CN 103632798 B CN103632798 B CN 103632798B CN 201310636021 A CN201310636021 A CN 201310636021A CN 103632798 B CN103632798 B CN 103632798B
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Abstract
The invention discloses a kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, by surface in situ synthetic method, nickel-zinc ferrite particle is coated with poly-3 methyl thiophene, reach the effect that poly-3 methyl thiophene firmly wraps up nickel-zinc ferrite nano particle, concrete employing coprecipitation first prepares nickel-zinc ferrite nano particle, nickel-zinc ferrite ionic ferrofluid is prepared subsequently with obtained nickel-zinc ferrite nano particle, 3 methyl thiophene monomer is added again and initator in-situ polymerization obtains poly-3 methyl thiophene good clad nano nickel-zinc ferrite magnetic particle in nickel-zinc ferrite ionic ferrofluid, finally prepare poly-3 methyl thiophene clad nano nickel-zinc ferrite magnetic particle magnetic liquid with nickel-zinc ferrite/poly-3 methyl thiophene composite particles.
Description
Technical field
The present invention relates to the preparation method of a kind of conducting polymer parcel nano magnetic particle magnetic liquid, particularly relate to a kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Background technology
Magnetic liquid refers to the colloidal solution of a kind of high stability that the nano magnetic particle highly dispersed that size magnitude is less than single magnetic domain is formed in liquid base load liquid, the dispersant of general magnetic liquid is organic polymer chain, do not possess special performance, and once after original nano magnetic particle and dispersant joining place superscribe one deck organic semiconductor in magnetic liquid, a kind of novel organic inorganic hybridization magnetic liquid just arises at the historic moment, organic semiconductor is by after organically combining with magnetic liquid, organic semi-conductor performance is just by regulating magnetic field intensity to make magnetic liquid possess regular photoelectric properties change, therefore such Magnetic Fluids has great potential in the application in the field such as micro-optic device and photonic crystal.
But the preparation of this kind of magnetic liquid needs to overcome three difficult points: one is the stability that conduction gathers 3 methyl thiophene coated magnetic Nano-Ferrite Particle; Two is the size magnitude control that conduction gathers 3 methyl thiophene integument; Three be parcel after nano magnetic particle how stable dispersion is in base load liquid.
Summary of the invention
The object of this invention is to provide a kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, improve the stability of the poly-3 methyl thiophene coated magnetic Nano-Ferrite Particle of conduction, control the size magnitude of the poly-3 methyl thiophene integument of conduction, make the nano magnetic particle stable dispersion after wrapping up in base load liquid.
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, above two kinds of solution is poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 20-30 minute, then Magneto separate 4-6 hour, spend deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution pours in the above-mentioned solution washed the 30-40 minute that seethes with excitement into, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into the nickel-zinc ferrite Massart magnetic liquid of 1-2%, slaking 6-8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3-4h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 24-26h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Advantage of the present invention is: the present invention is coated with poly-3 methyl thiophene by nano nickel Zn ferrite particle by surface in situ synthetic method, reach the effect that poly-3 methyl thiophene firmly wraps up nickel-zinc ferrite nano particle, by mathematical computations 3 methyl thiophene amount of monomer, be aided with polymerization inhibitor again and accurately control the degree of polymerization, the size magnitude preventing from the 3 methyl thiophene degree of polymerization from exceeding magnetic liquid carrying, control in 10-20 nanometer, thus reach the effect of control nickel-zinc ferrite/poly-3 methyl thiophene composite particles particle diameter, obtain magnetic liquid, also improve the stability (placing not sink for six months) of the poly-3 methyl thiophene coated magnetic Nano-Ferrite Particle of conduction simultaneously.This magnetic liquid is owing to there being one deck conducting polymer coating layer, therefore it is under the effect of regular variation magnetic field, its photoelectric properties aspect produce also can regularity change, namely the object regulating its performance index in photoelectricity of magnetic field intensity controllable adjustment is finally reached through, in the research of magnetic liquid, hew out the subbranch of novel a Gong research, there is very important Study and appliance and be worth.
Embodiment
Following case study on implementation is provided in conjunction with foregoing invention content.
Embodiment 1:
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, and above two kinds of solution are poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 20 minutes, then Magneto separate 4 hours, spends deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution washed and is seethed with excitement 30 minutes, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, and with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into 1% nickel-zinc ferrite Massart magnetic liquid, slaking 6 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 24h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 2:
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, and above two kinds of solution are poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 25 minutes, then Magneto separate 5 hours, spends deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution washed and is seethed with excitement 35 minutes, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, and with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into 1.5% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3.5h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 25h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 3:
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, and above two kinds of solution are poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 30 minutes, then Magneto separate 6 hours, spends deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution washed and is seethed with excitement 40 minutes, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, and with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into 2% nickel-zinc ferrite Massart magnetic liquid, slaking 8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 4h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 26h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 4:
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, and above two kinds of solution are poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 18 minutes, then Magneto separate 3 hours, spends deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution washed and is seethed with excitement 25 minutes, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, and with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into 1% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 2h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 20h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 5:
A kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, and above two kinds of solution are poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 35 minutes, then Magneto separate 7 hours, spends deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution washed and is seethed with excitement 45 minutes, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, and with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into 2% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 5h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 28h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
The poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid performance that each embodiment obtains is as shown in the table:
As can be seen from the above data, embodiment 1-3 within the scope of present invention process obtains the size magnitude that poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid can carry, control in 10-20 nanometer, well stability, obviously be better than in the extraneous embodiment 4,5 of present invention process, poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid performance prepared by the visible the present invention of have employed has good size magnitude and stability, has important using value.
Claims (1)
1. a preparation method for poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, is characterized by:
Its preparation method is:
A, 31.32gFe (NO
3)
39H
2o, 12.89gNi (NO
3)
26H
2o, 24.57gZn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24gFeSO
47H
2o is dissolved in 250ml water and is configured to solution, above two kinds of solution is poured in there-necked flask and adds 70mL concentrated ammonia liquor after dissolving, stir 20-30 minute, then Magneto separate 4-6 hour, spend deionized water to pH=7.0,82.02gFe (NO
3)
39H
2o is dissolved in 500ml water and is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution pours in the above-mentioned solution washed the 30-40 minute that seethes with excitement into, and Magneto separate, to naturally cooling to room temperature, outwells supernatant liquor, with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverizes, and obtains nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91mol.L
-1salpeter solution be made into the nickel-zinc ferrite Massart magnetic liquid of 1-2%, slaking 6-8 days;
C, add in beaker the Massart magnetic liquid prepared add water 100ml dilution mixture evenly after, 3ml3-methylthiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3-4h, and add 15% ammonium persulfate solution 20ml in period, reaction terminates rear Magneto separate, and after respectively washing three times with 0.8mol/l sulfuric acid and acetone, with acetone washing to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get that 1 restraint gets ready nickel-zinc ferrite/poly-3 methyl thiophene compound particle joins in the mixed solution of 0.8g cetyl benzenesulfonic acid sodium, 2ml90% ethanol and 8ml deionized water, after stirred at ambient temperature reaction 24-26h, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle with supercentrifuge centrifugal segregation, get its upper liquid and namely obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
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| US7560160B2 (en) * | 2002-11-25 | 2009-07-14 | Materials Modification, Inc. | Multifunctional particulate material, fluid, and composition |
| CN102627834A (en) * | 2012-04-05 | 2012-08-08 | 南昌航空大学 | Preparation method of chitosan modification barium ferrite filling multi-walled carbon nanotube/poly 3-methylthiophene composite wave-absorbing material |
| CN103632798A (en) * | 2013-12-03 | 2014-03-12 | 东华理工大学 | Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid |
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| US7560160B2 (en) * | 2002-11-25 | 2009-07-14 | Materials Modification, Inc. | Multifunctional particulate material, fluid, and composition |
| CN102627834A (en) * | 2012-04-05 | 2012-08-08 | 南昌航空大学 | Preparation method of chitosan modification barium ferrite filling multi-walled carbon nanotube/poly 3-methylthiophene composite wave-absorbing material |
| CN103632798A (en) * | 2013-12-03 | 2014-03-12 | 东华理工大学 | Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid |
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| 钕掺杂镍锌铁氧体-聚苯胺复合材料的制备;谢宇等;《航空科学基金》;20110131;第47页实验步骤部分，第48页透射电镜分析以及磁性初步分析部分 * |
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