CN101183590A - Malic acid coating water-based magnetic fluid material and production thereof - Google Patents
Malic acid coating water-based magnetic fluid material and production thereof Download PDFInfo
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- CN101183590A CN101183590A CNA200710046724XA CN200710046724A CN101183590A CN 101183590 A CN101183590 A CN 101183590A CN A200710046724X A CNA200710046724X A CN A200710046724XA CN 200710046724 A CN200710046724 A CN 200710046724A CN 101183590 A CN101183590 A CN 101183590A
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Abstract
The invention relates to a malic acid coated water-based magnetic fluid material and the preparation method of the material, belonging to the technical field of materials and the preparation. The water-based magnetic fluid material comprises a magnetic nanometer Fe3O4, a malic acid coated layer and carrier water; wherein, the grain diameter of the magnetic manometer particles is in the range from 8.9nm to 15.4nm and the saturation magnetization is in the range of 31emu/g to 45.6emu/g. In the invention, the namometer-sized Fe3O4 is prepared by chemical coprecipitation method, chemical bondings are generated between the carboxyl in the malic acid and the surfaces of Fe3O4 namometer particles and the a stable magnetic fluid is formed due to the coated malic acid which can prevent the aggregation of the nanometer particles. The invention has the advantages that: firstly, the prepared namometer Fe3O4 material is in a smaller size and a narrow distribution, the saturation magnetization is higher and the material is a favorable magnetic material; secondly, the operation method has the advantages of easy operation and low requirement of the instruments and experimental conditions, meanwhile, because of the low reaction temperature, oxygen is not necessarily isolated, thus, the environmental protection effect is favorable.
Description
Technical field
The present invention relates to a kind of water-based magnetic fluid material, especially relate to water-based magnetic fluid material of a kind of malic acid coating and preparation method thereof, belong to material and preparing technical field thereof.
Background technology
Magnetic fluid is a kind of intellectual material that controllable rheology is arranged that changes with externally-applied magnetic field, the ferromagnetism of its existing solid magnetic material, the flowability that liquid is arranged again, therefore successful Application in many fields such as space flight and aviation, electronics, chemical industry, machinery, the energy, metallurgy, biological medicine.
The type of magnetic fluid carrier fluid is selected according to sealing medium and operating mode, can be water, kerosene, silicone oil, mercury etc.Development along with Green Chemistry, water-based magnetic fluid has been avoided the pollution of organic solvent to environment, and water is harmless, and all magnetic fluids that are applied to biological medicine all are carrier fluid with water at present, so water-based magnetic fluid all has very important application prospects at aspects such as chemical industry, environmental protection, medical treatment.
The surfactant that is used to prepare water-based magnetic fluid at present mainly contains enuatrol, dodecyl sodium sulfate, polyethylene glycol, citric acid, sodium tartrate, polyacrylic acid, polyvinyl alcohol etc., and medical magnetic fluid will be considered the biocompatibility of coating layer, therefore normal some large biological molecules of selection such as n-capric acid, gelatin, cyclodextrin, glucan, amino acid etc.
It is surfactant that the present invention adopts malic acid, makes stable water-based magnetic fluid with chemical coprecipitation, and easy to operation and raw material is easy to get.
Summary of the invention
The object of the present invention is to provide a kind of water-based magnetic fluid material of malic acid coating of excellent performance.
Another object of the present invention is to provide the preparation method of the water-based magnetic fluid that a kind of malic acid easy and simple to handle, that environmental effect is good coats.
Water-based magnetic fluid of the present invention is made up of magnetic Nano Fe3O4, malic acid coating layer and carrier water, and wherein magnetic Nano Fe3O4 particle particle diameter is 8.9-15.4nm, and saturation magnetization is 31-45.6emu/g.
The preparation method of above-mentioned magnetic fluid adopts chemical coprecipitation to make, and its concrete processing step is as follows:
The first step, raw material are equipped with: ferric nitrate is mixed with the aqueous solution of 0.12-0.36mol/L, and ferrous sulfate is mixed with the aqueous solution of 0.08-0.24mol/L, malic acid is mixed with the aqueous solution of 0.17mol/L;
Second step, the preparation of nanometer Fe 3O4: the iron salt solutions for preparing is respectively got 10ml mix, in 40 ℃ of waters bath with thermostatic control, add 1.6-4.8ml ammoniacal liquor (25%), stir 15min, be warming up to 60 ℃ and stir 5min, stop reaction.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid;
The 3rd step, the preparation of magnetic fluid: in the precipitation of cleaning, add 16-48ml water, stir, ultrasonic, get the black uniform solution, be designated as solution A; Get the aqueous solution of malic acid that 4-12ml prepares, add 0.027-0.081g NaOH respectively, be designated as solution B.Solution B is added in the solution A, stir 6h, ultrasonic 2min, water-based magnetic fluid that must be stable.
The basic principle of the inventive method is: utilize chemical coprecipitation to prepare nanoscale Fe
3O
4, carboxyl energy and Fe in the malic acid
3O
4Nanoparticle surface generation chemical bonding, thus the malic acid that is coated on around the particle can stop the stable magnetic fluid of nano particle reunion formation.
The inventive method compared with prior art has the following advantages:
(1) the present invention adopts chemical coprecipitation to prepare Fe
3O
4, this method is easy and simple to handle, to instrument and experiment condition require low because reaction temperature is low, so need not starvation.
(2) nanometer Fe that makes
3O
4Particle diameter is little, and narrowly distributing, and it is stronger to have coated the saturation magnetization behind the malic acid, is good magnetic material.
(3) this magnetic fluid is a carrier fluid with water, is surfactant with the malic acid, and is all harmless to environment and human body, meets the requirement of Green Chemistry.
(4) raw material is easy to get, and is easy to commercial Application.
Embodiment
Embodiment 1: get the iron nitrate solution of 10ml 0.12mol/L and the copperas solution of 10ml 0.08mol/L, mixing also stirs, and in 40 ℃ of waters bath with thermostatic control, adds 1.6ml ammoniacal liquor (25%) fast, stir 15min, stop after being warming up to 60 ℃ of reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid, what obtain is exactly nanometer Fe
3O
4Add 16ml water in this precipitation, the ultrasonic 2min dark solution of homogeneous of loosing of can getting a point is designated as solution A; Get the aqueous solution of malic acid of 4ml 0.17mol/L, add 0.027g NaON, be stirred to dissolving fully, be designated as solution B.Solution B is added in the solution A, stir 6h both are fully acted on, ultrasonic 2min, finally water-based magnetic fluid that can be stable.The particle diameter of the Nano composite granules that this method makes is 8.9nm, and saturation magnetization is 3 1emu/g.
Embodiment 2: get the iron nitrate solution of 10ml 0.18mol/L and the copperas solution of 10ml 0.12mol/L, mixing also stirs, and in 40 ℃ of waters bath with thermostatic control, adds 2.4ml ammoniacal liquor (25%) fast, stir 15min, stop after being warming up to 60 ℃ of reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.Add 24ml water in this precipitation, the ultrasonic 2min dark solution of homogeneous of loosing of can getting a point is designated as solution A; Get the aqueous solution of malic acid of 6ml 0.17mol/L, add 0.04g NaOH, be stirred to dissolving fully, be designated as solution B.Solution B is added in the solution A, stir 6h, ultrasonic 2min, finally water-based magnetic fluid that can be stable.The particle diameter of the Nano composite granules that this method makes is 10.2nm, and saturation magnetization is 33.5emu/g.
Embodiment 3: get the iron nitrate solution of 10ml 0.24mol/L and the copperas solution of 10ml 0.16mol/L, mixing also stirs, and in 40 ℃ of waters bath with thermostatic control, adds 3.2ml ammoniacal liquor (25%) fast, stir 15min, stop after being warming up to 60 ℃ of reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.Add 32ml water in this precipitation, the ultrasonic 2min dark solution of homogeneous of loosing of can getting a point is designated as solution A; Get the aqueous solution of malic acid of 8ml 0.17mol/L, add 0.054g NaOH, be stirred to dissolving fully, be designated as solution B.Solution B is added in the solution A, stir 6h, ultrasonic 2min, finally water-based magnetic fluid that can be stable.The particle diameter of the Nano composite granules that this method makes is 12nm, and saturation magnetization is 36emu/g.
Embodiment 4: get the iron nitrate solution of 10ml 0.3mol/L and the copperas solution of 10ml 0.2mol/L, mix and stir, in 40 ℃ of waters bath with thermostatic control, add 4ml ammoniacal liquor (25%) fast, stir 15min, stop after being warming up to 60 ℃ of reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.Add 40ml water in this precipitation, the ultrasonic 2min dark solution of homogeneous of loosing of can getting a point is designated as solution A; Get the aqueous solution of malic acid of 10ml 0.17mol/L, add 0.068g NaOH, be stirred to dissolving fully, be designated as solution B.Solution B is added in the solution A, stir 6h, ultrasonic 2min, finally water-based magnetic fluid that can be stable.The particle diameter of the Nano composite granules that this method makes is 14.5nm, and saturation magnetization is 42emu/g.
Embodiment 5: get the iron nitrate solution of 10ml 0.36mol/L and the copperas solution of 10ml 0.24mol/L, mixing also stirs, and in 40 ℃ of waters bath with thermostatic control, adds 4.8ml ammoniacal liquor (25%) fast, stir 15min, stop after being warming up to 60 ℃ of reaction 5min.With the black precipitate that the distilled water washing generates, be neutral until supernatant liquid.Add 48ml water in this precipitation, the ultrasonic 2min dark solution of homogeneous of loosing of can getting a point is designated as solution A; Get the aqueous solution of malic acid of 12ml 0.17mol/L, add 0.081g NaOH, be stirred to dissolving fully, be designated as solution B.Solution B is added in the solution A, stir 6h, ultrasonic 2min, finally water-based magnetic fluid that can be stable.The particle diameter of the Nano composite granules that this method makes is 15.4nm, and saturation magnetization is 45.6emu/g.
Claims (2)
1. the water-based magnetic fluid material that malic acid coats is characterized in that being made up of magnetic Nano Fe3O4, malic acid coating layer and carrier water, and wherein magnetic Nano Fe3O4 particle particle diameter is 8.9-15.4nm, and saturation magnetization is 31-45.6emu/g.
2. the preparation method of the water-based magnetic fluid material that coats of a malic acid is characterized in that comprising following step:
The first step, raw material are equipped with: ferric nitrate is mixed with the aqueous solution of 0.12-0.36mol/L, and ferrous sulfate is mixed with the aqueous solution of 0.08-0.24mol/L, malic acid is mixed with the aqueous solution of 0.17mol/L;
Second step, the preparation of nanometer Fe 3O4: the iron salt solutions for preparing is respectively got 10ml mix, in 40 ℃ of waters bath with thermostatic control, add 1.6-4.8ml ammoniacal liquor (25%), stir 15min, be warming up to 60 ℃ and stir 5min, stop reaction, with the black precipitate that the distilled water washing generates, be neutral until supernatant liquid;
The 3rd step, the preparation of magnetic fluid: in the precipitation of cleaning, add 16-48ml water, stir, ultrasonic, get the black uniform solution, be designated as solution A; Get the aqueous solution of malic acid that 4-12ml prepares, add 0.027-0.081g NaOH respectively, be designated as solution B; Solution B is added in the solution A, stir 6h, ultrasonic 2min, water-based magnetic fluid that must be stable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710046724XA CN101183590A (en) | 2007-09-30 | 2007-09-30 | Malic acid coating water-based magnetic fluid material and production thereof |
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|---|---|---|---|
| CNA200710046724XA CN101183590A (en) | 2007-09-30 | 2007-09-30 | Malic acid coating water-based magnetic fluid material and production thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307192B (en) * | 2008-07-02 | 2011-04-06 | 北京航空航天大学 | Ferroferric oxide nanometer particles with excellent water dispersancy and method for preparing same |
| CN101882495B (en) * | 2009-05-09 | 2011-12-21 | 西北师范大学 | Nano Fe3O4/ polystyrene-maleic anhydride magnetic hybrid material and preparation method thereof |
| CN101901656B (en) * | 2009-12-24 | 2013-01-16 | 陕西北美基因股份有限公司 | Preparation method of magnetic particle with surface modified isothiocyanato active group |
| CN103273081A (en) * | 2013-05-31 | 2013-09-04 | 上海师范大学 | Process for preparing ferriferrous oxide magnetic fluid |
-
2007
- 2007-09-30 CN CNA200710046724XA patent/CN101183590A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307192B (en) * | 2008-07-02 | 2011-04-06 | 北京航空航天大学 | Ferroferric oxide nanometer particles with excellent water dispersancy and method for preparing same |
| CN101882495B (en) * | 2009-05-09 | 2011-12-21 | 西北师范大学 | Nano Fe3O4/ polystyrene-maleic anhydride magnetic hybrid material and preparation method thereof |
| CN101901656B (en) * | 2009-12-24 | 2013-01-16 | 陕西北美基因股份有限公司 | Preparation method of magnetic particle with surface modified isothiocyanato active group |
| CN103273081A (en) * | 2013-05-31 | 2013-09-04 | 上海师范大学 | Process for preparing ferriferrous oxide magnetic fluid |
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