CN103449534A - Method for preparing magnetic nanoparticle by using ionic liquid as template agent - Google Patents
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Abstract
The invention discloses a method for preparing a magnetic nanoparticle by using ionic liquid as a template agent. The method comprises the following steps of preparing a nanoscale magnetic Fe3O4 particle by using ionic liquid as the template agent and using FeSO4.7H2O and FeCl3.6H2O as materials through a chemical coprecipitation method; mixing the FeSO4.7H2O with FeCl3.6H2O, adding deionized water and then adding the ionic liquid template agent; stirring the mixture for 0.5-3 hours at the temperature of 40 DEG C-100 DEG C and at the stirring speed of 1200r/min, and adding ammonia water to adjust the pH value of the reactants to be 8-11, further stirring fiercely for 0.5-3 hours under the condition that the stirring speed is 1200r/min until the color of the reaction mixture is changed into black, and stopping the stirring; ultrasonically cleaning five times with the power of 200W, wherein cleaning at every time keeps 1 minute, separating the substances by a magnet after the cleaning is finshed, and vacuum drying for 7-12 hours at the temperature of 50 DEG C-100 DEG C. The Fe3O4 nanoparticle of the prepared magnetic nanoparticle is smaller in particle diameter and narrower in distribution, has superparamagnetism; the method has the characteristics of strong repeatability and low cost, and is simple and feasible.
Description
Technical field
The present invention relates to the nano material production technical field, particularly a kind ofly take ionic liquid and prepare the method for magnetic nano-particle as template.
Background technology
Magnetic nano-particle has more and more widely application in a lot of fields, and as aspect magnetic recording material, magnetic nano-particle can be used for preparing the high density magnetic recording material.At biological technical field, magnetic nano-particle can be used for DNA, protein and magnetic immuno cellular segregation.In addition, magnetic nano-particle can also be for nuclear magnetic resonance, and drug release is controlled etc.Magnetic nano-particle Fe
3o
4preparation method commonly used mainly contains two kinds: aqueous reaction coprecipitation method and high-temperature decomposition.Although aqueous reaction coprecipitation method commonly used is simple to operate and cost is low, the Fe prepared
3o
4nanoparticle shape is irregular, and size distribution is wider, and, because its specific surface is larger, is easy to cause the appearance of agglomeration.High-temperature decomposition is higher to equipment requirements, and temperature is wayward, and the reaction raw materials cost is large, strong toxicity, and product production is lower.Therefore, seek cost low, easy and simple to handle, and the preparation method of excellent product performance is the study hotspot received much attention at present.
Ionic liquid (Ionic Liquids) generally refers in room temperature and approaches the organic liquid material be comprised of ion fully under room temperature, also referred to as organic melting salt.It has that steam forces down, thermostability and chemical stability is high, liquid temperature wide ranges, solvability and the advantage such as catalytic activity is stronger, be that traditional volatility is high, the ideal substitute of the contaminate environment thing such as strong toxicity, inflammable, explosive organic solvent or highly corrosive solvent, be suitable for cleaning technique that current Green Chemistry advocates and the requirement of Sustainable development, more and more by the extensive recognition and acceptance of people.
In recent years, ionic liquid is because of its excellent physical and chemical performance, and the advantage in the inorganic nano-particle preparation also more and more receives people's concern.The ionic liquid surface tension is little, can make the nucleation rate of inorganic nano-particle uprise, and the nano particle diameter made thus is less.The ionic liquid surface can be low, can make material there is therein good stability, also strengthened different kinds of molecules dissolving power therein, ionic liquid can provide the polarity of hydrophobic group and high guidance quality, this polarity makes them can be parallel or perpendicular to the surface of dissolved material, is the equal of a template of substance reaction.In addition, ionic liquid can form the hydrogen bond of " prolongation " under liquid state, as entropy drive spontaneous form tissue well, the nanostructure of long-range order.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide and a kind ofly take ionic liquid as template prepares the method for magnetic nano-particle, can prepare particle diameter little, narrowly distributing and the Fe with superparamagnetism
3o
4nanoparticle, have easy and simple to handlely, and repeatability is strong, the characteristics that cost is low.
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind ofly take ionic liquid as template prepares the method for magnetic nano-particle, comprise following operation steps:
The first step: by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds the ionic liquid template;
Second step: said mixture is 40-100 ℃ in temperature, stir 0.5-3 hour under the condition that stirring velocity is 1200r/min, then add ammoniacal liquor to regulate the pH value of above-mentioned reactant to 8-11, then continue strong stirring 0.5-3 hour under the condition that low whipping speed is 1200r/min, until the color of reaction mixture becomes black, stop stirring;
The 3rd step: be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50-100 ℃ in temperature, vacuum-drying 7-12 hour, prepare magnetic nano-particle.
According to following operation steps, prepared by described ionic liquid template:
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed with n-propylcarbinyl chloride or the bromine band normal butane of 75mmol, reaction 7-24 hour at the temperature of 90-120 ℃, reacted product is through acetone or methylene dichloride recrystallization, make imidazoles bromine salt ion liquid or imidazoles villaumite ionic liquid, the ionic liquid made and the sodium tetrafluoroborate of 73mmol, sodium hexafluoro phosphate or two (trifluoromethane sulphonyl) imine lithium carry out anionresin, make the ionic liquid template with respective anionic.
Described ionic liquid template is 1-butyl-3-Methylimidazole villaumite [Bmim] Cl, 1-butyl-3-Methylimidazole bromine salt [Bmim] Br, 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4, 1-butyl-3-Methylimidazole hexafluorophosphate [Bmim] PF
6or any one in two (trifluoromethane sulphonyl) inferior amine salt [Bmim] TFSI of 1-butyl-3-Methylimidazole.
Described by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds in the ionic liquid template FeSO
47H
2o and FeCl
36H
2the mass ratio of O is 1:1-4; The consumption of deionized water is 30-100ml; The mass ratio of mixture and ionic liquid template is 0.5-6:100.
In the described magnetic nano-particle prepared, described magnetic nano-particle is Fe
3o
4.
Beneficial effect of the present invention is:
Preparation method of the present invention has easy and simple to handle, and repeatability is strong, the characteristics that cost is low.The Fe that uses method of the present invention to make
3o
4nano particle diameter is little, narrowly distributing and have superparamagnetism.
The accompanying drawing explanation
The Fe that Fig. 1 is embodiment 1 preparation
3o
4the XRD figure of nanoparticle.
The Fe that Fig. 2 is embodiment 1 preparation
3o
4the SEM figure of nanoparticle.
The Fe that Fig. 3 is embodiment 1 preparation
3o
4the hysteresis curve of nanoparticle.
Embodiment
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
A kind ofly take ionic liquid as template prepares the method for magnetic nano-particle, comprise following operation steps:
The first step: by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds the ionic liquid template;
Second step: said mixture is 40-100 ℃ in temperature, stir 0.5-3 hour under the condition that stirring velocity is 1200r/min, then add ammoniacal liquor to regulate the pH value of above-mentioned reactant to 8-11, then continue strong stirring 0.5-3 hour under the condition that low whipping speed is 1200r/min, until the color of reaction mixture becomes black, stop stirring;
The 3rd step: be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50-100 ℃ in temperature, vacuum-drying 7-12 hour, prepare magnetic nano-particle.
According to following operation steps, prepared by described ionic liquid template:
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed with n-propylcarbinyl chloride or the bromine band normal butane of 75mmol, reaction 7-24 hour at the temperature of 90-120 ℃, reacted product is through acetone or methylene dichloride recrystallization, make imidazoles bromine salt ion liquid or imidazoles villaumite ionic liquid, the ionic liquid made and the sodium tetrafluoroborate of 73mmol, sodium hexafluoro phosphate or two (trifluoromethane sulphonyl) imine lithium carry out anionresin, make the ionic liquid template with respective anionic.
Described ionic liquid template is 1-butyl-3-Methylimidazole villaumite [Bmim] Cl, 1-butyl-3-Methylimidazole bromine salt [Bmim] Br, 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4, 1-butyl-3-Methylimidazole hexafluorophosphate [Bmim] PF
6or any one in two (trifluoromethane sulphonyl) inferior amine salt [Bmim] TFSI of 1-butyl-3-Methylimidazole.
Described by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds in the ionic liquid template FeSO
47H
2o and FeCl
36H
2the mass ratio of O is 1:1-4; The consumption of deionized water is 30-100ml; The mass ratio of mixture and ionic liquid template is 0.5-6:100.
Referring to accompanying drawing, the Fe that Fig. 1 is embodiment 1 preparation
3o
4the XRD figure of nanoparticle; The Fe that Fig. 2 is embodiment 1 preparation
3o
4the SEM figure of nanoparticle; The Fe that Fig. 3 is embodiment 1 preparation
3o
4the hysteresis graph of nanoparticle.
XRD analysis is to carry out on the D/max2200pc diffractometer of producing in Rigaku company (Rigaku), is furnished with the Cu target
.From XRD spectra, the Fe of preparation
3o
4nanoparticle is face-centred cubic structure, and crystal formation is better, does not find other impurity.SEM figure shows the Fe of preparation
3o
4nanoparticle is better dispersed, and median size is in the 20nm left and right.The Fe that Fig. 3 is embodiment 1 preparation
3o
4the hysteresis curve of nanoparticle.As can be seen from Figure 3, under room temperature, without hysteresis, without remanent magnetism, without coercive field, saturation magnetization is 60.66emu/g, and sample has superparamagnetism preferably.
Embodiment 1
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, the imidazoles villaumite ionic liquid obtained and the sodium tetrafluoroborate of 73mmol carry out anionresin, make ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:1 according to mass ratio is mixed, then adds in the 70ml deionized water, and the mixture then made adds ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF according to the ratio of mass ratio 3:100
4; Said mixture is to stir 0.5 hour under 70 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 8 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 0.5 hour, until the color of reaction mixture becomes black, stop stirring; The ultrasonic cleaning that is 200W with power 5 times, clean 1 minute each time, and the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, the magnetic nano-particle Fe prepared
3o
4.
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, the imidazoles villaumite ionic liquid obtained and the sodium hexafluoro phosphate of 73mmol carry out anionresin, make ionic liquid template 1-butyl-3-Methylimidazole hexafluorophosphate [Bmim] PF
6.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:1 according to mass ratio is mixed, then adds in the 70ml deionized water, and the mixture then made adds ionic liquid template 1-butyl-3-Methylimidazole hexafluorophosphate [Bmim] PF according to the ratio of mass ratio 3:100
6; Said mixture is to stir 0.5 hour under 70 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 8 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 0.5 hour, until the color of reaction mixture becomes black, stop stirring; Be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, prepares magnetic nano-particle Fe
3o
4.
Embodiment 3
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, two (trifluoromethane sulphonyl) imine lithiums of the imidazoles villaumite ionic liquid obtained and 73mmol carry out anionresin, make two (trifluoromethane sulphonyl) inferior amine salt [Bmim] TFSI of ionic liquid template 1-butyl-3-Methylimidazole.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:1 according to mass ratio is mixed, then adds in the 70ml deionized water, and the mixture then made adds two (trifluoromethane sulphonyl) inferior amine salt [Bmim] TFSI of ionic liquid template 1-butyl-3-Methylimidazole according to the ratio of mass ratio 3:100; Said mixture is to stir 0.5 hour under 70 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 8 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 0.5 hour, until the color of reaction mixture becomes black, stop stirring; Be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, prepares magnetic nano-particle Fe
3o
4.
Embodiment 4
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, the imidazoles villaumite ionic liquid obtained and the sodium tetrafluoroborate of 73mmol carry out anionresin, make ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:2 according to mass ratio is mixed, then adds in the 80ml deionized water, and the mixture then made adds ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF according to the ratio of mass ratio 4:100
4; Said mixture is to stir 1 hour under 80 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 9 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 1 hour, until the color of reaction mixture becomes black, stop stirring; Be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, the magnetic nano-particle Fe prepared
3o
4.
Embodiment 5
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, the imidazoles villaumite ionic liquid obtained and the sodium tetrafluoroborate of 73mmol carry out anionresin, make ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:3 according to mass ratio is mixed, then adds in the 90ml deionized water, and the mixture then made adds ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF according to the ratio of mass ratio 5:100
4; Said mixture is to stir 2 hours under 90 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 10 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 2 hours, until the color of reaction mixture becomes black, stop stirring; Be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, prepares magnetic nano-particle Fe
3o
4.
Embodiment 6
(1) preparation of ionic liquid template
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed at the temperature of 90 ℃ with the n-propylcarbinyl chloride of 75mmol, react 7 hours; Reacted product is through acetone recrystallization, separate out white solid, it is 1-butyl-3-Methylimidazole villaumite ionic liquid, the imidazoles villaumite ionic liquid obtained and the sodium tetrafluoroborate of 73mmol carry out anionresin, make ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4.
(2) magnetic nano-particle Fe
3o
4preparation
By FeSO
47H
2o and FeCl
36H
2the ratio that O is 1:4 according to mass ratio is mixed, then adds in the 100ml deionized water, and the mixture then made adds ionic liquid template 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF according to the ratio of mass ratio 6:100
4; Said mixture is to stir 3 hours under 100 ℃, the stirring velocity condition that is 1200r/min in temperature, then regulate the pH value to 11 of above-mentioned reactant with ammoniacal liquor, then under the condition that low whipping speed is 1200r/min, continue strong stirring 3 hours, until the color of reaction mixture becomes black, stop stirring; Be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50 ℃ in temperature, vacuum-drying is 7 hours, prepares magnetic nano-particle Fe
3o
4.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (5)
1. take ionic liquid as template prepares the method for magnetic nano-particle for one kind, it is characterized in that, comprise following operation steps:
The first step: by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds the ionic liquid template;
Second step: said mixture is 40-100 ℃ in temperature, stir 0.5-3 hour under the condition that stirring velocity is 1200r/min, then add ammoniacal liquor to regulate the pH value of above-mentioned reactant to 8-11, then continue strong stirring 0.5-3 hour under the condition that low whipping speed is 1200r/min, until the color of reaction mixture becomes black, stop stirring;
The 3rd step: be 200W ultrasonic cleaning 5 times with power, clean each time 1 minute, the material after having cleaned separates with magnet, and under the condition that is 50-100 ℃ in temperature, vacuum-drying 7-12 hour, prepare magnetic nano-particle.
2. according to claim 1ly a kind ofly take ionic liquid as template prepares the method for magnetic nano-particle, it is characterized in that, prepared according to following operation steps by described ionic liquid template:
At N
2in the compression ring border, the N-Methylimidazole of 75mmol is mixed with n-propylcarbinyl chloride or the bromine band normal butane of 75mmol, reaction 7-24 hour at the temperature of 90-120 ℃, reacted product is through acetone or methylene dichloride recrystallization, make imidazoles bromine salt ion liquid or imidazoles villaumite ionic liquid, the ionic liquid made and the sodium tetrafluoroborate of 73mmol, sodium hexafluoro phosphate or two (trifluoromethane sulphonyl) imine lithium carry out anionresin, make the ionic liquid template with respective anionic.
3. according to claim 1 and 2ly a kind ofly take ionic liquid and prepare the method for magnetic nano-particle as template, it is characterized in that: described ionic liquid template is 1-butyl-3-Methylimidazole villaumite [Bmim] Cl, 1-butyl-3-Methylimidazole bromine salt [Bmim] Br, 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF
4, 1-butyl-3-Methylimidazole hexafluorophosphate [Bmim] PF
6or any one in two (trifluoromethane sulphonyl) inferior amine salt [Bmim] TFSI of 1-butyl-3-Methylimidazole.
4. according to claim 1ly a kind ofly take ionic liquid as template prepares the method for magnetic nano-particle, it is characterized in that: described by FeSO
47H
2o and FeCl
36H
2o mixes, and adds deionized water, then adds in the ionic liquid template FeSO
47H
2o and FeCl
36H
2the mass ratio of O is 1:1-4; The consumption of deionized water is 30-100ml; The mass ratio of mixture and ionic liquid template is 0.5-6:100.
5. according to claim 1ly a kind ofly take ionic liquid and prepare the method for magnetic nano-particle as template, it is characterized in that: described magnetic nano-particle is Fe
3o
4.
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| CN104030363A (en) * | 2014-02-17 | 2014-09-10 | 瑞安市浙工大技术转移中心 | Preparing method of ferroferric oxide nanometer particles |
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| RU2572418C1 (en) * | 2014-10-16 | 2016-01-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Северный (Арктический) федеральный университет имени М.В. Ломоносова" (САФУ) | Method of producing magnetoactive compound |
| CN105366733A (en) * | 2015-12-01 | 2016-03-02 | 江南大学 | Preparation method for rodlike Fe3O4 in ionic liquid |
| CN105753067A (en) * | 2016-01-26 | 2016-07-13 | 三明学院 | Grain size adjusting method of superparamagnetic iron oxide microspheres |
| CN106800315A (en) * | 2017-01-17 | 2017-06-06 | 上海交通大学 | A kind of ionic liquid assisted microwave synthesis radiation method synthesizes the method for extra small magnetic Nano cluster |
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| CN104030363A (en) * | 2014-02-17 | 2014-09-10 | 瑞安市浙工大技术转移中心 | Preparing method of ferroferric oxide nanometer particles |
| CN104030363B (en) * | 2014-02-17 | 2016-05-25 | 瑞安市浙工大技术转移中心 | A kind of preparation method of ferriferrous oxide nano-particle |
| RU2572418C1 (en) * | 2014-10-16 | 2016-01-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Северный (Арктический) федеральный университет имени М.В. Ломоносова" (САФУ) | Method of producing magnetoactive compound |
| CN104386760A (en) * | 2014-10-31 | 2015-03-04 | 山东师范大学 | Method for rapidly preparing magnetic carrier material in large quantity |
| CN104386760B (en) * | 2014-10-31 | 2015-12-30 | 山东师范大学 | A kind of rapid, high volume prepares the method for magnetic carrier material |
| CN105366733A (en) * | 2015-12-01 | 2016-03-02 | 江南大学 | Preparation method for rodlike Fe3O4 in ionic liquid |
| CN105753067A (en) * | 2016-01-26 | 2016-07-13 | 三明学院 | Grain size adjusting method of superparamagnetic iron oxide microspheres |
| CN105753067B (en) * | 2016-01-26 | 2017-05-24 | 三明学院 | Grain size adjusting method of superparamagnetic iron oxide microspheres |
| CN106800315A (en) * | 2017-01-17 | 2017-06-06 | 上海交通大学 | A kind of ionic liquid assisted microwave synthesis radiation method synthesizes the method for extra small magnetic Nano cluster |
| CN106800315B (en) * | 2017-01-17 | 2018-02-02 | 上海交通大学 | A kind of method that ionic liquid assisted microwave synthesis radiation method synthesizes extra small magnetic Nano cluster |
| CN108910961A (en) * | 2018-09-03 | 2018-11-30 | 谢燕青 | A kind of preparation method of ferroso-ferric oxide |
| CN112742349A (en) * | 2019-10-30 | 2021-05-04 | 中石化南京化工研究院有限公司 | For CO2Trapped magnetic ionic liquid nano composite adsorption material |
| CN111437792A (en) * | 2020-04-13 | 2020-07-24 | 山东建筑大学 | Synthetic method of magnetic mesoporous silica for removing copper ions in water |
| CN111437792B (en) * | 2020-04-13 | 2023-03-03 | 山东建筑大学 | Synthetic method of magnetic mesoporous silica for removing copper ions in water |
| CN115475656A (en) * | 2022-09-05 | 2022-12-16 | 河南科技大学 | Preparation method of magnetic solid acid and application of magnetic solid acid in biomass hydrolysis |
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