CN100446134C - Method for preparing iron-oxide particle suspension - Google Patents
Method for preparing iron-oxide particle suspension Download PDFInfo
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- CN100446134C CN100446134C CNB2006101181137A CN200610118113A CN100446134C CN 100446134 C CN100446134 C CN 100446134C CN B2006101181137 A CNB2006101181137 A CN B2006101181137A CN 200610118113 A CN200610118113 A CN 200610118113A CN 100446134 C CN100446134 C CN 100446134C
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Abstract
The invention involves in a kind of preparation method of ferric oxide particlue suspensolid. First of all the invention uses deposition oxidation method to prepare the magnetic particles of 3~100 nano under the condition of ultrasonic wave, and the surfactant is added to cover the magnetic particles whilst when they are being prepared, and then disperse them into water by mixing and ultrasonic wave treatment, finally the ferric oxide suspensoid is made. The said magnetic particle is ferroferric oxide or gamma ferric oxide. The invention is of simple technology, the ferric oxide particle it is made by this way is of good biological compatibility and good stability of suspensoid, additionally there is no deposition or aggregation in 10 minutes after the suspensoid is operated by centrifugal force with a rotate speed of 9000RPM; and no deposition of magnetic particles is found after it is stored at the room temperature for 180 days. The suspensoid is of good alternating magnetic field heating effect: the temperature of 1 milliliter of suspensoid containing 10 milligrammers ferroferric oxide will rise by 74 C degree by heating 3 minutes after it is put in the alternating magnetic field of 20 kiloampere/meter field strength and 55 khz frequency.
Description
Technical field
What the present invention relates to is the method for a kind of medical material tech field preparation, specifically is a kind of preparation method of the stable iron-oxide particle suspension with very strong alternating magnetic field heating effect.
Background technology
To be a class ferromagnetism or magnetic nano-particle stably be scattered in colloidal solution in the carrier fluid by surfactant to magnetic suspension liquid, and its magnetic fluid under alternating magnetic field can be converted into heat energy with magnetic energy.The magnetic thermotherapy is to utilize this characteristic and a kind of novel thermotherapy means that grow up.Thermotherapy obtains clinical practice already as a kind of method of adjuvant therapy of tumors, and it is to utilize various physical means that the tumor tissues temperature is risen to more than 43 ℃, and keeps a period of time, relies on the sensitiveness of tumour cell to heat, quickens cancer cell death.Therefore, magnetic suspension liquid becomes the focus of thermotherapy research gradually.
But the effect of present employed magnetic suspension liquid thermotherapy is also not very good, mainly be because magnetic particle heating effect wherein is lower, be difficult for the temperature of tumor tissues is heated to more than 43 ℃, and the dispersion stabilization of magnetic suspension liquid is also not so good, reunite after placing a period of time, thereby cause heating effect obviously to reduce.In addition, the biocompatibility of the surfactant that magnetic suspension liquid is adopted is also bad, limits its application in human body.Therefore, new magnetic particle preparation method constantly explores, and various surfactants with excellent biological compatibility also are applied gradually simultaneously.
Find that through the literature search to prior art the Chinese patent publication number is CN 1410137A, name is called: thermotherapy nano-magnetic seed and its production and use.This patent disclosure a kind of thermotherapy preparation method with magnetic suspension liquid, it is that the nano-magnetic powder of certain proportioning and surfactant are added in the pure water, obtains magnetic suspension liquid by abundant dispersion, can be used for the thermotherapy treatment tumour.But the used magnetic particle of this method is nano-magnetic powders such as nanometer ferromagnetism magnetic, nanometer ferrimagnetism magnetic and nano-magnetic magnetic, and its heat production ability is not high, can influence the effect of thermotherapy; And be after the nano-magnetic powder preparation is finished, to mix with surfactant and water again, disperseing, the stable of the suspension that this process for dispersing is made usually poorly reunite easily, and the concentration of dispersion liquid is not high yet, influences the effect of thermotherapy; Simultaneously, the surfactant that this method adopted is softex kw and calgon etc., and these surfactants have certain toxicity, can produce toxic and side effect to human body.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method of iron-oxide particle suspension is provided.The iron-oxide particle suspension excellent in stability of the present invention preparation, and this suspension has good alternating magnetic field heating effect, can not produce toxic and side effect to human body simultaneously.
The present invention is achieved by the following technical solutions, the present invention at first adopts the precipitation oxidizing process to prepare tri-iron tetroxide or the gamma-Fe2O3 equimagnetic particle that diameter is the 3-100 nanometer under the ultrasonic wave effect, adding surfactant in preparation coats magnetic particle, adopt stirring and ultrasonic Treatment to be distributed in the water at last, obtain having the magnetic suspension liquid of advantages of excellent stability and heating effect.
Below method of the present invention is done further to limit, step is as follows:
(1) preparation of magnetic particle: coat surfactant tri-iron tetroxide or gamma-Fe2O3 magnetic particles such as covering glucan with precipitation oxidizing process synthetic surface under action of ultrasonic waves, the preparation method is as follows:
0.05 mole divalent iron salt, 0.04 mole of oxidant and 2 gram surfactants are dissolved in the 200 gram water are mixed with the aqueous solution, add in the there-necked flask; Other is dissolved in 0.1 mole alkali in the 100 gram water, is mixed with the aqueous solution.Drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make the tri-iron tetroxide particle of clad surface activating agent, covering amount is the 5%-50% of magnetic particle.
Ferriferrous oxide nano-particle and oxidant were reacted 2 hours under 40 ℃ of temperature again and obtain the gamma-Fe2O3 particle.
Can regulate between the 3-100 nanometer with the tri-iron tetroxide of method for preparing and the average grain diameter of gamma-Fe2O3 particle, the specific saturation magnetization of the particle of preparing should should be less than 900e greater than 20emu/g, coercive force, and particle size distribution is even.The covering amount of surfactant is the 5%-50% of magnetic particle.
(2) preparation of suspension: will add in the entry through the magnetic particle of clad surface activating agent, stirring and ultrasonic dispersion in 5-30 minute through 10-60 minute obtain the magnetic particle suspension of concentration in the 1%-20% scope.
Magnetic particle of the present invention mainly is tri-iron tetroxide or gamma-Fe2O3 particle.
Divalent iron salt of the present invention can be a kind of in ferrous sulfate, the frerrous chloride etc.
Oxidant of the present invention can be a kind of in potassium nitrate, sodium nitrate, hydrogen peroxide, pure oxygen, the air etc.
Surfactant of the present invention can be a kind of of surfactants such as glucan, shitosan, polyethylene glycol, PLA.
Alkali of the present invention can be a kind of in NaOH, potassium hydroxide, ammoniacal liquor, the urea etc.
Dispersion of the present invention, its medium are pure water or physiological saline.
The present invention selects for use tri-iron tetroxide or gamma-Fe2O3 nano particle as the heat production material, in the preparation process of magnetic particle, adopt ultrasonic Treatment, and used the surfactant with excellent biological compatibility magnetic particle is dispersed in the water, prepared a kind of stable iron-oxide particle suspension with strong alternating magnetic field heating effect.The medicine that tri-iron tetroxide or gamma-Fe2O3 nano particle are made is used widely clinical, confirms that it has excellent biological compatibility, can not bring toxic and side effect to human body as other magnetic materials.And the tri-iron tetroxide or the gamma-Fe2O3 particle of the present invention preparation be nano level, but the more micron-sized magnetic particle of its heat production rate is higher in this yardstick.In addition,, specially select surfactants such as glucan for use, therefore can guarantee these surfactant excellent biological compatibility in clinical practice for avoiding bringing toxic and side effect.Select for use surfactants such as glucan also good compatibility to be arranged with glassware for drinking water, iron oxide particles is carried out can significantly increasing after the surface treatment hydrophily of particle with them, make it stable dispersion in water, prepare the good magnetic suspension liquid of high concentration and dispersion stabilization.The most outstanding characteristics of the present invention are to adopt ultrasonic wave to handle in tri-iron tetroxide for preparing dextran-coated with the precipitation oxidizing process or gamma-Fe2O3 nano particle process; Use ultrasonic wave to handle when dextran-coated, its most outstanding advantage can significantly improve tri-iron tetroxide or gamma-Fe2O3 particle heat production ability: compare with the iron oxide particles of conventional method preparation, its heat production ability can improve 2-4 doubly.
Compared with prior art, the present invention has the following advantages: (1) preparation is simple: raw materials used is the common chemical medicine, cheap; Technological process is simple, and the reaction condition gentleness.(2) can regulate in the 3-100 nanometer range with the magnetic particle diameter of the present invention's preparation, and particle size distribution is less, can be in the medium-term and long-term evenly dispersion of water.(3) the magnetic particle that coats of the surfactant that adopts with the present invention can evenly, stably be dispersed in the water, has good stability, does not find the sedimentation or the reunion of magnetic particle after centrifugal 10 minutes with 9000 rev/mins rotating speed; At room temperature store the sedimentation of also not finding the magnetic particle in 180 days.(4) suspension made from the present invention has very strong alternating magnetic field heating effect.Placing field intensity with 1 milliliter of suspension that contains 10 milligrams, 4 milligrams and 2 milligrams tri-iron tetroxide particles respectively is 20 kilo-ampere/rice, frequency is that 55 kilo hertzs alternating magnetic field heated 3 minutes, its temperature has risen 74 ℃, 45 ℃ and 26 ℃ respectively, demonstrates very good alternating magnetic field heating effect.(5) material of surfactant used in the present invention for being used widely at biomedicine field can not produce toxic and side effect to human body.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
4.6 gram potassium nitrate, 2 gram glucans and 14.08 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 60 minutes, use ultrasonic dispersion 30 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 2
4.6 gram potassium nitrate, 4 gram glucans and 13.96 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then that product is extremely neutral with deionized water wash, making average grain diameter is the dextran-coated tri-iron tetroxide particle of 3-5 nanometer.Get 10 this particles of gram and add in 50 gram physiological saline, stirred 60 minutes, use ultrasonic dispersion 20 minutes then, make concentration and be 20% magnetic particle suspension.
Embodiment 3
4.6 gram potassium nitrate, 8 gram glucans and 14.14 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then that product is extremely neutral with deionized water wash, making average grain diameter is the dextran-coated tri-iron tetroxide particle of 100 nanometers.Get 1 this particle of gram and add in 99 gram pure water, stirred 30 minutes, use ultrasonic dispersion 30 minutes then, make concentration and be 1% magnetic particle suspension.
Embodiment 4
1.4 gram hydrogen peroxide, 2 gram glucans and 5.98 gram frerrous chlorides are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 60 minutes, use ultrasonic dispersion 10 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 5
4.6 gram potassium nitrate, 2 gram shitosans and 14.08 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain ammoniacal liquor with 1.7 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 10 minutes, use ultrasonic dispersion 5 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 6
4.9 gram sodium nitrate, 8 gram glucans and 14.08 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 10 minutes, use ultrasonic dispersion 30 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 7
4.6 gram potassium nitrate, 3 gram PLAs and 14.08 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain NaOH with 4 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 60 minutes, use ultrasonic dispersion 20 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 8
4.6 gram potassium nitrate, 1 gram glucan, 1 gram shitosan and 14.08 gram ferrous sulfate are dissolved in the 200 gram water, add in the there-necked flask; Restrain potassium hydroxide with 5.6 in addition and be dissolved in the 100 gram water, drip ferric ion solutions in the there-necked flask under ultrasonic wave and stirring action, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection.Then with product with deionized water wash to neutral, make average grain diameter and be the dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram pure water, stirred 60 minutes, use ultrasonic dispersion 30 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 9
Making average grain diameter according to embodiment 1 described method is dextran-coated tri-iron tetroxide particle about 10 nanometers.Get 5 this particles of gram and add in 45 gram physiological saline, stirred 60 minutes, use ultrasonic dispersion 30 minutes then, make concentration and be 10% magnetic particle suspension.
Embodiment 10
Making average grain diameter according to embodiment 1 described method is dextran-coated tri-iron tetroxide particle about 10 nanometers, adds in the there-necked flask, adds hydrogen peroxide again, reacts 2 hours under 40 ℃ of temperature again and obtains gamma-Fe2O3.Making concentration according to embodiment 1 described method then is 10% magnetic particle suspension.
Embodiment 11
Making average grain diameter according to embodiment 1 described method is dextran-coated tri-iron tetroxide particle about 10 nanometers, adds in the there-necked flask, and aerating oxygen again reacted 2 hours under 40 ℃ of temperature again and obtains the gamma-Fe2O3 particle.Making concentration according to embodiment 1 described method then is 10% magnetic particle suspension.
The average diameter of selecting the foregoing description preparation for use is that the suspension (concentration is 10%) of tri-iron tetroxide particle of the dextran-coated of 10 nanometers heats experiment: placing field intensity with 1 milliliter of suspension that contains 10 milligrams, 4 milligrams and 2 milligrams tri-iron tetroxide particles respectively is 20 kilo-ampere/rice, frequency is that 55 kilo hertzs alternating magnetic field heated 3 minutes, its temperature has risen 74 ℃, 45 ℃ and 26 ℃ respectively, demonstrates good alternating magnetic field heating effect.
Claims (8)
1, a kind of preparation method of iron-oxide particle suspension is characterized in that:
The first step: synthesize the tri-iron tetroxide or the gamma-Fe2O3 particle of clad surface activating agent that diameter is the magnetic of 3-100 nanometer: 0.05 mole divalent iron salt, 0.04 mole of oxidant and 2 gram surfactants are dissolved in the 200 gram water are mixed with the aqueous solution, add in the there-necked flask with the precipitation oxidizing process; Other is dissolved in 0.1 mole alkali in the 100 gram water, be mixed with the aqueous solution, under ultrasonic wave and stirring action, drip in the there-necked flask, produce precipitation, after waiting to dropwise, temperature of reaction system is risen to 90 ℃, reaction is 4 hours under stirring and nitrogen protection, then with product with deionized water wash to neutral, make the tri-iron tetroxide particle of clad surface activating agent; Perhaps tri-iron tetroxide particle and the oxidant with the clad surface activating agent reacts the gamma-Fe2O3 particle that obtained the clad surface activating agent in 2 hours again under 40 ℃ of temperature;
Second step: adopt stirring and ultrasonic Treatment to be distributed in the water, obtain iron-oxide particle suspension through the tri-iron tetroxide or the gamma-Fe2O3 particle of clad surface activating agent.
2, the preparation method of iron-oxide particle suspension according to claim 1, it is characterized in that, in described second step: the tri-iron tetroxide or the gamma-Fe2O3 particle of clad surface activating agent are added in the entry, disperse through 10-60 minute stirring and 5-30 minute ultrasonic wave, obtain the iron-oxide particle suspension of concentration in the 1%-20% scope.
3, the preparation method of iron-oxide particle suspension according to claim 1 is characterized in that, described divalent iron salt is a kind of in ferrous sulfate, the frerrous chloride.
4, the preparation method of iron-oxide particle suspension according to claim 1 is characterized in that, described alkali is a kind of in NaOH, potassium hydroxide, ammoniacal liquor, the urea.
5, the preparation method of iron-oxide particle suspension according to claim 1 is characterized in that, described oxidant is potassium nitrate, sodium nitrate, hydrogen peroxide, pure oxygen, airborne a kind of.
6, the preparation method of iron-oxide particle suspension according to claim 1 is characterized in that, described surfactant, be in glucan, shitosan, polyethylene glycol, the PLA one or more.
7, the preparation method of iron-oxide particle suspension according to claim 1, it is characterized in that, described dispersion is to adopt stirring and ultrasonic Treatment to be distributed in the pure water through the tri-iron tetroxide or the gamma-Fe2O3 particle of clad surface activating agent, obtains iron-oxide particle suspension.
8, the preparation method of iron-oxide particle suspension according to claim 1, it is characterized in that, described tri-iron tetroxide and gamma-Fe2O3 particle through the clad surface activating agent, its average grain diameter is between the 3-100 nanometer, the specific saturation magnetization of particle greater than 20emu/g, coercive force less than 90Oe, and particle size distribution is even, and the covering amount of surfactant is the 5%-50% of particle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US9745442B2 (en) | 2011-05-13 | 2017-08-29 | Korea Atomic Energy Research Institute | Epoxy resin composition for neutron shielding, and method for preparing the same |
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| 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 |
| EP2575772A4 (en) | 2010-05-26 | 2014-03-19 | Gen Hospital Corp | Magnetic nanoparticles |
| CN102502876A (en) * | 2011-10-11 | 2012-06-20 | 安徽明珠颜料科技有限公司 | Method for synthesizing iron oxide black by oxidizing sodium nitrate |
| CN103323586A (en) * | 2013-06-14 | 2013-09-25 | 中国科学院苏州生物医学工程技术研究所 | Blood platelet magnetizing and immunolabeling analysis method |
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| CN1214716A (en) * | 1996-04-10 | 1999-04-21 | 新材料公共服务公司研究所 | Process for preparing agglomerate-free nanoscalar iron oxide particles with hydrolysis-resistant coating |
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Cited By (1)
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| US9745442B2 (en) | 2011-05-13 | 2017-08-29 | Korea Atomic Energy Research Institute | Epoxy resin composition for neutron shielding, and method for preparing the same |
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