CN103632800B - A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid - Google Patents
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid Download PDFInfo
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- CN103632800B CN103632800B CN201310636131.4A CN201310636131A CN103632800B CN 103632800 B CN103632800 B CN 103632800B CN 201310636131 A CN201310636131 A CN 201310636131A CN 103632800 B CN103632800 B CN 103632800B
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Abstract
The invention discloses a kind of Fe3O4The preparation method that cladding polyaniline prepares magnetic fluid, first adopt Massart magnetic liquid as presoma again with polyaniline-coated, and with this Massart magnetic liquid, ethanol, aniline, sulphuric acid and anhydrous p-aminobenzene sulfonic acid for raw material, hydrothermal synthesis method is adopted to prepare the composite of ferrite cladding polyaniline, then pass through local reduction way, prepare the magnetic liquid of ferrite cladding polyaniline. This composite has good magnetic and stability, all has important using value in aviation, medical treatment, new material etc.
Description
Technical field
The present invention relates to a kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, belongs to electromagnetic wave absorbent material preparation field.
Background technology
Magnetic liquid is due to complicated process of preparation, and application is wide, in the world that the research of magnetic liquid is still very active at present. Constantly having new application to be found, new application technology is suggested, if nano-magnetic fluid is medically especially the application in the fields such as anti-curing oncoma and nano-magnetic fluid application on new energy development are all current study hotspots. External magnetic fluid, through the development of more than 40 years, has had very ripe commercial magnetic fluid and application product. The each bound pair nano magnetic material pay attention to day by day of current Chinese society, in the research of magnetic liquid technology, have been achieved for some break through, some scientific research institutions such as Beijing Iron and Steel Research Geueral Inst, Dalian University of Technology, Nanjing University, Beijing Institute of Aeronautics, Tongji University etc. carry out in this respect and have carried out fruitful research work, simultaneously domestic also form Ji Jia industrialization manufacturer, but due to evening of starting to walk, research and development strength is disperseed, and also has suitable gap compared with developed countries.
Summary of the invention
It is an object of the present invention to provide a kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, first adopt Massart magnetic liquid as presoma again with polyaniline-coated, and with this Massart magnetic liquid, ethanol, aniline, sulphuric acid and anhydrous p-aminobenzene sulfonic acid for raw material, hydrothermal synthesis method is adopted to prepare the composite of ferrite cladding polyaniline, then pass through local reduction way, prepare the magnetic liquid of ferrite cladding polyaniline. This magnetic fluid has good conduction and magnetic property.
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 50-70min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 25-35min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 2.5-3.5h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 0.9-1.1mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 22-26h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
The present invention is from numerous organic-capping materials being adopted, there is the polyaniline of good biocompatibility and stability, because of advantages such as its unique chemical property, mechanism of doping effect, high temperature resistant and antioxygenic property and excellent electrochromisms, become the first-selection of this experiment organic-capping material, in addition Fe3O4The magnetic property of nano-particle, makes to prepare doped polyaniline cladding Fe3O4Magnetic fluid is possibly realized. The magnetic fluid of preparation has good conduction and magnetic property, has important using value in fields such as aviation and medical treatment.
Detailed description of the invention
The invention will be further described by the examples below.
Embodiment 1:
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 50min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 25min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 2.5h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 0.9mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 22h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
Embodiment 2:
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 60min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 30min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 3h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 1.0mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 24h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
Embodiment 3:
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 70min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 35min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 3.5h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 1.1mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 26h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
Embodiment 4:
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 45min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 20min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 2h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 0.8mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 20h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
Embodiment 5:
A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 80min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 40min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 4h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 1.2mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 28h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
The polyaniline-coated Fe that embodiment 1-5 prepares3O4The magnetic property of magnetic fluid is as shown in the table:
| Conductivity | Saturation magnetization | Coercivity | |
| Embodiment 1 | 5.278 S/cm | 0.18 emu/g | 58.3 Oe |
| Embodiment 2 | 5.797 S/cm | 0.25 emu/g | 53.8 Oe |
| Embodiment 3 | 5.451 S/cm | 0.21 emu/g | 61.0 Oe |
| Embodiment 4 | 4.139 S/cm | 0.09 emu/g | 70.7 Oe |
| Embodiment 5 | 4.342 S/cm | 0.11 emu/g | 72.6 Oe |
As can be seen from the above data, embodiment 1-3 within the scope of present invention process prepares the magnetic property of magnetic fluid and is substantially better than in the extraneous embodiment 4,5 of present invention process, especially with the best results of embodiment 2, magnetic fluid prepared by the visible present invention of have employed has good conduction and magnetic property, has important using value.
Claims (2)
1. a polyaniline-coated Fe3O4The preparation method of magnetic fluid, is characterized by:
Preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 50-70min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 25-35min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 2.5-3.5h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 0.9-1.1mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 22-26h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
2. a polyaniline-coated Fe3O4The preparation method of magnetic fluid, is characterized by:
Its preparation method is:
(1) nanometer Fe3O4Preparation:
31.32gFe (NO3)3·9H2O water dissolution is configured to Fe (NO to 250ml3)3·9H2O solution, 12.24gFeSO4·7H2O water dissolution is configured to FeSO to 250ml4·7H2O solution, Fe (NO3)3·9H2O solution and FeSO4·7H2O solution is poured into and is added 50mL strong aqua ammonia after in three-neck flask, stops, separating with Magnet under room temperature after stirring reaction 60min, outwell the supernatant, with deionized water cyclic washing until neutrality, remove supernatant, cleaning twice with benzophenone, normal temperature drying grinds and obtains nanometer Fe again3O4Particle;
(2) Fe3O4The preparation of Massart magnetic liquid:
Take 9g nanometer Fe3O4Particle joins the Fe (NO of 500ml0.1mol/L3)3Mixing in solution, be again heated to boiling 30min, rear wait solution is cooled to room temperature, after washing drying and grinding with water, adds the salpeter solution of 95.45ml0.081468mol/L, stands one day, obtain Massart magnetic liquid;
(3) polyaniline-coated Fe3O4The preparation of magnetic ion:
Beaker add after the Massart magnetic liquid prepared adds water to 50ml mix homogeneously, again anhydrous to 0.75ml aniline, 2ml sulphuric acid and 0.01g p-aminobenzene sulfonic acid is added in beaker, ice-water bath 3h, and add ammonium persulfate solution in period, ammonium persulfate solution is the configuration of 1.87g Ammonium persulfate. water dissolution to 20ml to be formed, and reaction terminates rear sucking filtration, and after respectively washing three times with 1.0mol/l sulphuric acid and acetone, with deionized water wash to pH=7, obtain Fe3O4/ PANI compound particle;
(4) polyaniline-coated Fe3O4The preparation of magnetic fluid:
The Fe that will prepare3O4/ PANI compound particle joins in the mixed solution of 50ml0.5mol/l dodecylbenzene sodium sulfonate and 50ml0.5mol/l ethanol, under room temperature after stirring reaction 24h, fails homodisperse Fe with high speed centrifuge centrifugal segregation3O4/ PANI compound particle, takes its upper liquid and namely obtains polyaniline-coated Fe3O4Magnetic fluid.
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