CN103632800A - Method for preparing polyaniline coated Fe3O4 magnetic fluid - Google Patents

Method for preparing polyaniline coated Fe3O4 magnetic fluid Download PDF

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CN103632800A
CN103632800A CN201310636131.4A CN201310636131A CN103632800A CN 103632800 A CN103632800 A CN 103632800A CN 201310636131 A CN201310636131 A CN 201310636131A CN 103632800 A CN103632800 A CN 103632800A
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polyaniline
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CN103632800B (en
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乐长高
谢宇
潘建飞
谢宗波
黄彦
李凤
曾繁山
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East China Institute of Technology
Nanchang Hangkong University
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Nanchang Hangkong University
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Abstract

The invention discloses a method for preparing magnetic fluid through coating Fe3O4 with polyaniline. According to the method, Massart magnetic liquid is firstly adopted as a precursor and then is coated with polyaniline, a polyaniline coated ferrite composite material is prepared from the Massart magnetic liquid, ethanol, aniline, sulfuric acid and anhydrous sulfanilic acid, which serve as raw materials, by adopting a hydrothermal synthesis method, and then, polyaniline coated ferrite magnetic liquid is prepared by an in-situ reduction method. The composite material has good magnetism and stability and has an important application value in the aspects of aviation, medical treatment, novel materials and the like.

Description

A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid
Technical field
The present invention relates to a kind of polyaniline-coated Fe 3o 4the 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, at present still very active to the research of magnetic liquid in the world.Constantly have new application to be found, new application technology is suggested, and as nano-magnetic fluid, special application and the application of nano-magnetic fluid on new energy development in the fields such as anti-curing oncoma in medical treatment is all current study hotspot.External magnetic fluid, through the development of more than 40 years, has had very ripe commercial magnetic fluid and application product.Current each bound pair nano magnetic material pay attention to day by day of Chinese society, aspect the research of magnetic liquid technology, obtaining some breakthroughs, some scientific research institutions have carried out fruitful research work 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, the domestic Liao Jijia industrialization manufacturer that also forms simultaneously, but because starting is late, research and development strength is disperseed, and also has suitable gap compared with developed countries.
Summary of the invention
The object of the invention is to provide a kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, first adopt Massart magnetic liquid to use again polyaniline-coated as presoma, and to take this Massart magnetic liquid, ethanol, aniline, sulfuric acid and anhydrous sulfanilic acid be raw material, adopt hydrothermal synthesis method to prepare the composite material of the coated polyaniline of ferrite, then by local reduction way, prepare the magnetic liquid of the coated polyaniline of ferrite.This magnetic fluid has good conduction and magnetic property.
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 50-70min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 25-35min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 2.5-3.5h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 0.9-1.1mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 22-26h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
The present invention is from the numerous organic-capping materials that can be adopted, there is good biocompatibility and the polyaniline of stability, because of its unique chemical property, mechanism of doping effect, high temperature resistant and antioxygenic property and the good advantages such as electrochromism, become the first-selection of this experiment organic-capping material, in addition Fe 3o 4the magnetic property of nano particle, makes to prepare the coated Fe of doped polyaniline 3o 4magnetic fluid becomes possibility.The magnetic fluid of preparation has good conduction and magnetic property, in fields such as aviation and medical treatment, has important using value.
Embodiment
Below by embodiment, the invention will be further described.
Embodiment 1:
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 50min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 25min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 2.5h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 0.9mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 22h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
Embodiment 2:
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 60min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 30min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 3h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 1.0mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 24h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
Embodiment 3:
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 70min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 35min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 3.5h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 1.1mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 26h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
Embodiment 4:
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 45min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 20min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 2h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 0.8mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 20h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
Embodiment 5:
A kind of polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 80min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 40min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 4h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 1.2mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 28h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
The polyaniline-coated Fe that embodiment 1-5 makes 3o 4the magnetic property of magnetic fluid is as shown in the table:
? Conductance Saturation magnetization Coercive force
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, the magnetic property that embodiment 1-3 in processing range of the present invention makes magnetic fluid is obviously better than the embodiment 4,5 outside processing range of the present invention, especially with the best results of embodiment 2, the visible magnetic fluid that has adopted the present invention to prepare has good conduction and magnetic property, has important using value.

Claims (3)

1. a polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, is characterized by: preparation method comprises nanometer Fe 3o 4preparation, Fe 3o 4the preparation of Massart magnetic liquid, polyaniline-coated Fe 3o 4the preparation of magnetic ion, polyaniline-coated Fe 3o 4four steps of preparation of magnetic fluid.
2. a polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, is characterized by:
Preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 50-70min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 25-35min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 2.5-3.5h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 0.9-1.1mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 22-26h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
3. a polyaniline-coated Fe 3o 4the preparation method of magnetic fluid, is characterized by:
Its preparation method is:
(1) nanometer Fe 3o 4preparation:
31.32g Fe (NO 3) 39H 2o water is dissolved to 250ml and is configured to Fe (NO 3) 39H 2o solution, 12.24g FeSO 47H 2o water is dissolved to 250ml and is configured to FeSO 47H 2o solution, Fe (NO 3) 39H 2o solution and FeSO 47H 2o solution adds 50 mL concentrated ammonia liquors after pouring in three-neck flask, under room temperature, after stirring reaction 60min, stop, separated with magnet, outwell supernatant liquor, use deionized water cyclic washing until neutrality is removed supernatant, with benzophenone, clean twice again, air drying grinds and obtains nanometer Fe 3o 4particle;
(2) Fe 3o 4the preparation of Massart magnetic liquid:
Get 9g nanometer Fe 3o 4particle joins the Fe (NO of 500ml 0.1 mol/L 3) 3in solution, mix, then be heated to the 30min that seethes with excitement, rear wait solution is cooled to room temperature, washes with water after drying and grinding, adds the salpeter solution of 95.45ml 0.081468 mol/L, standing one day, obtains Massart magnetic liquid;
(3) polyaniline-coated Fe 3o 4the preparation of magnetic ion:
After adding the Massart magnetic liquid having prepared to add water to 50ml in beaker to mix, again 0.75ml aniline, 2ml sulfuric acid and the anhydrous sulfanilic acid of 0.01g are added in beaker, ice-water bath 3h, and during add ammonium persulfate solution, ammonium persulfate solution is 1.87g ammonium persulfate water to be dissolved to 20ml configuration form, and reaction finishes rear suction filtration, and respectively washes after three times with 1.0mol/l sulfuric acid and acetone, with deionized water, wash to pH=7, obtain Fe 3o 4/ PANI compound particle;
(4) polyaniline-coated Fe 3o 4the preparation of magnetic fluid:
By the Fe preparing 3o 4/ PANI compound particle joins in the mixed solution of 50ml 0.5mol/l neopelex and 50ml 0.5mol/l ethanol, under room temperature after stirring reaction 24h, with the centrifugal removal of supercentrifuge, fails homodisperse Fe 3o 4/ PANI compound particle, gets its upper strata liquid and obtains polyaniline-coated Fe 3o 4magnetic fluid.
CN201310636131.4A 2013-12-03 2013-12-03 A kind of polyaniline-coated Fe3O4The preparation method of magnetic fluid Expired - Fee Related CN103632800B (en)

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CN105023693A (en) * 2015-07-28 2015-11-04 南昌航空大学 Preparation method of polyaniline-coated nano-composite magnetic liquid
JP7046298B1 (en) * 2021-07-21 2022-04-04 南京大学 Methods for Accelerating Startup of Anaerobic Reactors Based on Conductive Nanomaterials

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Publication number Priority date Publication date Assignee Title
CN105023693A (en) * 2015-07-28 2015-11-04 南昌航空大学 Preparation method of polyaniline-coated nano-composite magnetic liquid
JP7046298B1 (en) * 2021-07-21 2022-04-04 南京大学 Methods for Accelerating Startup of Anaerobic Reactors Based on Conductive Nanomaterials

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