CN101206944A - Method of preparing bioavailability water-based magnetofluid - Google Patents
Method of preparing bioavailability water-based magnetofluid Download PDFInfo
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- CN101206944A CN101206944A CNA2007100475424A CN200710047542A CN101206944A CN 101206944 A CN101206944 A CN 101206944A CN A2007100475424 A CNA2007100475424 A CN A2007100475424A CN 200710047542 A CN200710047542 A CN 200710047542A CN 101206944 A CN101206944 A CN 101206944A
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Abstract
The invention relates to a biological compatible water-based magnetic fluid material and the preparation method thereof, and belongs to the fields of the material and the preparation technology thereof. In the invention, nanometer scale Fe3O4 particles are prepared by adopting a chemical coprecipitation method in common use and dispersed in water, the surface modification is performed to the nanometer scale Fe3O4 particles with gluconic acid sodium salt, and finally stable water-based magnetic fluid is obtained. The magnetic fluid prepared by adopting the method of the invention takes Fe3O4 as the magnetic material, the gluconic acid sodium salt as a coating layer, and water as a carrier, thus the magnetic fluid has good biological compatibility. During the preparation process, oxygen is not required to be isolated, the particle diameter of the obtained Fe3O4 is small, and the distribution is narrow. In addition, the preparation method has the advantages that raw materials are easy to be obtained, and the method is simple and easy to be carried out and widely applied.
Description
Technical field
The present invention relates to a kind of bioavailability water-based magnetofluid material and preparation method thereof, belong to material and preparing technical field thereof.
Background technology
To be a class ferromagnetism or superparamagnetic nanoparticle stably be dispersed in colloidal solution in the carrier fluid by surfactant or coating material to magnetic fluid.Under action of alternating magnetic field, this colloidal solution can promptly be converted into heat energy with magnetic energy owing to produce the relaxation loss.In recent years, the researcher in medical science and materialogy field utilizes this peculiar property to develop a kind of novel tumor treatment technology-tumour magnetic thermotherapy technology, and progressively moves towards clinical practice.
At present, mainly containing these 3 kinds of magnetic materials of polymer magnetic bead, magnetic liposome and bioavailability water-based magnetofluid is applied in the tumour magnetic thermotherapy.In above-mentioned material, polymer magnetic bead particle diameter is big and the shell biocompatibility is undesirable, and magnetic liposome ground stability is bad, so be difficult to be applied to clinical.Water-based magnetic fluid as the thermotherapy material have heat imitate property significantly, characteristics such as biocompatibility and good stability, therefore become important research direction in the magnetic thermotherapy.
The eighties in last century, the Jordan group of Germany has prepared the water-based magnetic fluid that disperses with glucan, and has obtained curative effect preferably in the body of animal on the thermotherapy.Subsequently, have a variety of bioavailability water-based magnetofluids of different surfaces activating agent that adopted successfully to be prepared again, the main surfactant that uses has polyethylene glycol, n-capric acid, pantothenic acid, cyclodextrin and some amino acidses.
It is surfactant that the present invention adopts gluconic acid sodium salt, makes stable water-based magnetic fluid with chemical coprecipitation, and easy to operation and raw material is easy to get.Gluconic acid sodium salt is a kind of good food additives and nutrition fortifier, also is applied to medical aspect, and nontoxic pollution-free can be by the human homergy, so this water-based magnetic fluid has excellent biological compatibility, can be used as the pyromagnetic treatment material of tumour.
Summary of the invention
The object of the present invention is to provide a kind of bioavailability water-based magnetofluid material.
Another object of the present invention is to provide a kind of preparation method of easy and simple to handle, water-based magnetic fluid that environmental effect is good.
Bioavailability water-based magnetofluid of the present invention is made up of magnetic Nano Fe3O4, gluconic acid sodium salt coating layer and carrier water, and wherein magnetic Nano Fe3O4 particle particle diameter is 8.7-15.4nm, and saturation magnetization is 35.3-43.6emu/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, gluconic acid sodium salt 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 sodium gluconate aqueous solution that 4-12ml prepares, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, water-based magnetic fluid that must be stable down at 40 ℃.
The basic principle of the inventive method is: utilize chemical coprecipitation to prepare nanoscale Fe
3O
4Hydroxyl energy and Fe in the gluconic acid sodium salt
3O
4Nanoparticle surface generation chemical bonding, thus the gluconic acid sodium salt that is coated on around the particle can stop the stable magnetic fluid of nano particle reunion formation again.
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 gluconic acid sodium salt, is good magnetic material.
(3) this magnetic fluid is a carrier fluid with water, is surfactant with the gluconic acid sodium salt, and is all harmless to environment and human body, meets the requirement of Green Chemistry, has excellent biological compatibility.
(4) raw material is easy to get, and is easy to extensive use.
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 sodium gluconate aqueous solution of 4ml 0.17mol/L, be designated as solution B.Solution B is added in the solution A, stir 2h down at 40 ℃ 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 8.7nm, and saturation magnetization is 35.3emu/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 sodium gluconate aqueous solution of 6ml 0.17mol/L, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, finally water-based magnetic fluid that can be stable down at 40 ℃.The particle diameter of the Nano composite granules that this method makes is 10nm, and saturation magnetization is 36.5emu/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 sodium gluconate aqueous solution of 8ml 0.17mol/L, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, finally water-based magnetic fluid that can be stable down at 40 ℃.The particle diameter of the Nano composite granules that this method makes is 12nm, and saturation magnetization is 38emu/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 sodium gluconate aqueous solution of 10ml 0.17mol/L, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, finally water-based magnetic fluid that can be stable down at 40 ℃.The particle diameter of the Nano composite granules that this method makes is 14.5nm, and saturation magnetization is 41.3emu/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 sodium gluconate aqueous solution of 12ml 0.17mol/L, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, finally water-based magnetic fluid that can be stable down at 40 ℃.The particle diameter of the Nano composite granules that this method makes is 15.4nm, and saturation magnetization is 43.6emu/g.
Claims (2)
1. a bioavailability water-based magnetofluid is characterized in that by magnetic Nano Fe
3O
4, gluconic acid sodium salt coating layer and carrier water forms, magnetic Nano Fe wherein
3O
4The particle particle diameter is 8.7-15.4nm, and saturation magnetization is 35.3-43.6emu/g.
2. the preparation method of a bioavailability water-based magnetofluid adopts chemical coprecipitation, it 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, gluconic acid sodium salt 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 sodium gluconate aqueous solution that 4-12ml prepares, be designated as solution B.Solution B is added in the solution A, stir 2h, ultrasonic 2min, water-based magnetic fluid that must be stable down at 40 ℃.
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| CN2007100475424A CN101206944B (en) | 2007-10-29 | 2007-10-29 | Method of preparing bioavailability water-based magnetofluid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102215608A (en) * | 2010-04-10 | 2011-10-12 | 太仓市铭铨环保节能科技有限公司 | Nano heating agent used for tumor millimeter wave thermotherapy and preparation method thereof |
| CN103083674A (en) * | 2012-12-05 | 2013-05-08 | 江南大学 | Method for preparing cyclodextrin grafted polymaleic anhydride magnetic nanoparticles |
| CN106698654A (en) * | 2016-12-21 | 2017-05-24 | 浙江工业大学 | Method for using Fe3O4/C to alleviate MBR membrane pollution |
-
2007
- 2007-10-29 CN CN2007100475424A patent/CN101206944B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102215608A (en) * | 2010-04-10 | 2011-10-12 | 太仓市铭铨环保节能科技有限公司 | Nano heating agent used for tumor millimeter wave thermotherapy and preparation method thereof |
| CN102215608B (en) * | 2010-04-10 | 2013-07-03 | 东莞市龙记环保科技有限公司 | Nano heating agent used for tumor millimeter wave thermotherapy and preparation method thereof |
| CN103083674A (en) * | 2012-12-05 | 2013-05-08 | 江南大学 | Method for preparing cyclodextrin grafted polymaleic anhydride magnetic nanoparticles |
| CN103083674B (en) * | 2012-12-05 | 2015-04-08 | 江南大学 | Method for preparing cyclodextrin grafted polymaleic anhydride magnetic nanoparticles |
| CN106698654A (en) * | 2016-12-21 | 2017-05-24 | 浙江工业大学 | Method for using Fe3O4/C to alleviate MBR membrane pollution |
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| CN101206944B (en) | 2010-09-01 |
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