CN103632798A - Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid - Google Patents
Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid Download PDFInfo
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Abstract
The invention discloses a method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid. According to the method, nickel-zinc ferrite particles are coated with poly-3-methylthiophene by a surface in-situ synthesis method, so as to reach the effect that nickel-zinc ferrite nanoparticles are firmly wrapped by poly-3-methylthiophene; the method specifically comprises the steps of firstly preparing the nickel-zinc ferrite nanoparticles by adopting a coprecipitation method, then, preparing nickel-zinc ferrite ionic magnetic liquid from the prepared nickel-zinc ferrite nanoparticles, then, carrying out in-situ polymerization by adding 3-methylthiophene monomers and an initiator into the nickel-zinc ferrite ionic magnetic liquid so as to obtain nickel-zinc ferrite magnetic nanoparticles which are excellently coated by poly-3-methylthiophene, and finally, preparing the poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid from nickel-zinc ferrite/poly-3-methylthiophene composite particles.
Description
Technical field
The present invention relates to a kind of preparation method of conducting polymer parcel nano magnetic particle magnetic liquid, relate in particular 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 nano magnetic particle highly dispersed that size magnitude is less than single magnetic domain in liquid base load liquid and the colloidal solution of a kind of high stability forming, the dispersant of general magnetic liquid is organic polymer chain, do not possess special performance, once and superscribe after one deck organic semiconductor at original nano magnetic particle and dispersant joining place 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 just can change by regulating magnetic field intensity to make magnetic liquid possess regular photoelectric properties, therefore such Magnetic Fluids has great potential in the application in the fields such as micro-optic device and photonic crystal.
But the preparation of this class magnetic liquid need to overcome three difficult points: the one, and the stability of the poly-3 methyl thiophene coated magnetic Nano-Ferrite Particle of conduction; The 2nd, the size magnitude of the poly-3 methyl thiophene integument of conduction is controlled; The 3rd, how stable dispersion is in base load liquid for the nano magnetic particle after parcel.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, improved 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, made nano magnetic particle stable dispersion after parcel in the base load liquid.
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 20-30 minute, and then the separated 4-6 hour of magnetic, washs to pH=7.0 with deionized water, 82.02g Fe (NO
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured the 30-40 minute that seethes with excitement in the above-mentioned solution having washed into, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverize, obtain nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91 mol.L
-1salpeter solution be made into the nickel-zinc ferrite Massart magnetic liquid of 1-2%, slaking 6-8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3-4h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 24-26h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and 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 again polymerization inhibitor and accurately control the degree of polymerization, prevent that the 3 methyl thiophene degree of polymerization from surpassing the size magnitude that magnetic liquid can carry, be controlled at 10-20 nanometer, thereby reach the effect of control nickel-zinc ferrite/poly-3 methyl thiophene composite particles particle diameter, obtain magnetic liquid, also improved the stability (place and do 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 also produce can regularity change, finally reach by regulating its object in the performance index aspect photoelectricity of magnetic field intensity controllable adjustment, the subbranch that has hewed out novel a Gong research in the research of magnetic liquid, has very important research and using value.
Embodiment
In conjunction with foregoing invention content, provide following case study on implementation.
Embodiment 1:
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 20 minutes, and then magnetic is separated 4 hours, washs to pH=7.0,82.02g Fe (NO with deionized water
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution having washed and is seethed with excitement 30 minutes, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing, until neutrality is 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 94.47ml0.91 mol.L
-1salpeter solution be made into 1% nickel-zinc ferrite Massart magnetic liquid, slaking 6 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 24h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 2:
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 25 minutes, and then magnetic is separated 5 hours, washs to pH=7.0,82.02g Fe (NO with deionized water
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution having washed and is seethed with excitement 35 minutes, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing, until neutrality is 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 94.47ml0.91 mol.L
-1salpeter solution be made into 1.5% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3.5h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 25h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 3:
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 30 minutes, and then magnetic is separated 6 hours, washs to pH=7.0,82.02g Fe (NO with deionized water
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution having washed and is seethed with excitement 40 minutes, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing, until neutrality is 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 94.47ml0.91 mol.L
-1salpeter solution be made into 2% nickel-zinc ferrite Massart magnetic liquid, slaking 8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 4h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 26h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 4:
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 18 minutes, and then magnetic is separated 3 hours, washs to pH=7.0,82.02g Fe (NO with deionized water
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution having washed and is seethed with excitement 25 minutes, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing, until neutrality is 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 94.47ml0.91 mol.L
-1salpeter solution be made into 1% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 2h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 20h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
Embodiment 5:
A poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 35 minutes, and then magnetic is separated 7 hours, washs to pH=7.0,82.02g Fe (NO with deionized water
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured in the above-mentioned solution having washed and is seethed with excitement 45 minutes, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing, until neutrality is 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 94.47ml0.91 mol.L
-1salpeter solution be made into 2% nickel-zinc ferrite Massart magnetic liquid, slaking 6-8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 5h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 28h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and 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 makes is as shown in the table:
As can be seen from the above data, embodiment 1-3 in processing range of the present invention makes the size magnitude that poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid can carry, be controlled at 10-20 nanometer, temperature is good, obviously be better than the embodiment 4,5 outside processing range of the present invention, adopt poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid performance prepared by the present invention to there is good size magnitude and stability as seen, had important using value.
Claims (2)
1. a poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, it is characterized by: adopt coprecipitation first to prepare nickel-zinc ferrite nano particle, with obtained nickel-zinc ferrite nano particle, prepare nickel-zinc ferrite ionic ferrofluid subsequently, in nickel-zinc ferrite ionic ferrofluid, add again 3 methyl thiophene monomer and initator in-situ polymerization to obtain the poly-good clad nano nickel-zinc ferrite of 3 methyl thiophene magnetic particle, finally with nickel-zinc ferrite/poly-3 methyl thiophene composite particles, prepare poly-3 methyl thiophene clad nano nickel-zinc ferrite magnetic particle magnetic liquid.
2. a preparation method for poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid, is characterized by:
Its preparation method is:
A, 31.32g Fe (NO
3)
39H
2o, 12.89g Ni (NO
3)
26H
2o, 24.57g Zn (NO
3)
26H
2o is dissolved in 250ml water and is configured to solution, then 12.24g FeSO
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 added 70 mL concentrated ammonia liquors after dissolving, stirs 20-30 minute, and then the separated 4-6 hour of magnetic, washs to pH=7.0 with deionized water, 82.02g Fe (NO
3)
39H
2o is dissolved in and in 500ml water, is configured to Fe (NO
3)
39H
2o solution, Fe (NO
3)
39H
2o solution is poured the 30-40 minute that seethes with excitement in the above-mentioned solution having washed into, and magnetic is separated to and naturally cools to room temperature, outwells supernatant liquor, with deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverize, obtain nano nickel Zn ferrite particle;
B, get 5 grams of above-mentioned steps gained nano nickel Zn ferrite particles, add 94.47ml0.91 mol.L
-1salpeter solution be made into the nickel-zinc ferrite Massart magnetic liquid of 1-2%, slaking 6-8 days;
C, in beaker, add the Massart magnetic liquid having prepared to add water 100ml dilution to mix after, 3ml 3 methyl thiophene, 0.8ml sulfuric acid and the anhydrous sulfanilic acid of 1g are added in beaker, ice-water bath 3-4h, and during add 15% ammonium persulfate solution 20ml, it is separated that reaction finishes rear magnetic, and respectively wash after three times with 0.8mol/l sulfuric acid and acetone, with acetone, wash to PH=7, obtain nickel-zinc ferrite/poly-3 methyl thiophene compound particle;
D, get the nickel-zinc ferrite that 1 restraint gets ready/poly-3 methyl thiophene compound particle and join in the mixed solution of 0.8g cetyl benzene sulfonic acid sodium salt, 2ml 90% ethanol and 8ml deionized water, under room temperature after stirring reaction 24-26h, with the centrifugal removal of supercentrifuge, fail homodisperse nickel-zinc ferrite/poly-3 methyl thiophene compound particle, get its upper strata liquid and obtain poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid.
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Cited By (3)
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| CN104291433A (en) * | 2014-10-15 | 2015-01-21 | 济南大学 | Method for treating organic waste water based on polythiophene/zero-valent iron composite material activated molecule oxygen |
| CN105161246A (en) * | 2015-08-21 | 2015-12-16 | 盐城工学院 | Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof |
| CN103632798B (en) * | 2013-12-03 | 2016-02-24 | 东华理工大学 | A kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid |
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| 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 |
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| CN103632798B (en) * | 2013-12-03 | 2016-02-24 | 东华理工大学 | A kind of preparation method of 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103632798B (en) * | 2013-12-03 | 2016-02-24 | 东华理工大学 | A kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid |
| CN104291433A (en) * | 2014-10-15 | 2015-01-21 | 济南大学 | Method for treating organic waste water based on polythiophene/zero-valent iron composite material activated molecule oxygen |
| CN104291433B (en) * | 2014-10-15 | 2016-03-02 | 济南大学 | A kind of method based on Polythiophene/zero-valent iron composite material activate molecular oxygen process organic waste water |
| CN105161246A (en) * | 2015-08-21 | 2015-12-16 | 盐城工学院 | Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof |
| CN105161246B (en) * | 2015-08-21 | 2017-05-10 | 盐城工学院 | Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof |
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