CN103666446A - Method of improving water-solubility of nano material and multifunctional nano material with improved water-solubility - Google Patents
Method of improving water-solubility of nano material and multifunctional nano material with improved water-solubility Download PDFInfo
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Abstract
The invention discloses a method of improving water-solubility of a nano material. The method comprises the following steps: S10, dissolving nano-particles into an organic solvent to prepare liquor A; S20, adding derivative liquor of graphene oxide into the liquor A, and uniformly mixing to obtain liquor B; S30, after carrying out centrifugal separation onto a water-phase layer in liquor B, cleaning an obtained solid by water and drying to obtain multifunctional nano material with improved water-solubility. The multifunctional nano material with improved water-solubility, which is obtained by the method for improving water-solubility of nano material disclosed by the invention, has good water solubility and multi-functionality, is not easy to agglomerate in a polar solvent and biological buffer liquor, and is relatively low in toxicity, therefore, harm is not generated on a living body.
Description
Technical field
The present invention relates to nano material, relate in particular to and a kind ofly improve the water miscible method of nano material and improve the multi-functional nanometer material after water-soluble by the method.
Background technology
Inorganic nano-particle refers to that microtexture has one dimension at least in nanoscale scope or the various ultra-fine particles that consist of as elementary cell them, such as quantum dot (QDs), nm gold particles (AuNPs), up-conversion fluorescence nanoparticle (UCNPs), ferroferric oxide magnetic nanoparticle (Fe in three-dimensional space
3o
4) etc.Compare with macroscopical body material, nanoparticle has unique quantum effect, small-size effect, surface effects and macroscopic quantum effect, thereby the excellent performance such as light, sound, electricity, magnetic, heat that shows many Size dependences, makes its prospect that is widely used in fields such as catalysis, electronics, optics, sensing, biology, medical science, material, national defence.Up to the present, the method for preparing nanoparticle that people have adopted has: coprecipitation method, physical grinding method, sol-gel method, solvent-thermal method, thermal decomposition method, microemulsion method etc.
But in can synthesizing the method for the less and better performances of particle diameter, using many solvents is all organic solvent, thereby what obtain is all hydrophobic nanoparticle, cannot meet it in the application of biological field.In the synthetic method of having reported, many documents all can carry out certain modification to the surface tissue of nanoparticle, improve the activity of nanoparticle, improve nanoparticle dispersiveness, surfactivity, functional and and other materials between compatible.The approach of modifying is mainly to adopt silicon-dioxide and some hydrophilic molecules, polymkeric substance (as thiohydracrylic acid, thioglycolic acid, polyacrylic acid, polyethyene diamine, polyoxyethylene glycol etc.) and biomolecules (as amino acid, polypeptide etc.) decorated nanometer particle surface, to strengthen the dispersiveness of particle in polar solvent.Yet the resulting particle of these methods using is at present reunited than being easier in polar solvent and biological buffer, and these polymkeric substance are also more expensive, and some polymkeric substance toxicity is larger.In this simultaneously, how the nanoparticle set of various functions is obtained to have multifunctional nano composite material in one, in preparation method, be still worth improvement and bring new ideas.
Summary of the invention
The present invention aims to provide a kind of water miscible method of nano material of improving, and the multi-functional nanometer material improving after water-soluble by this method is not easy to reunite in polar solvent and biological buffer, and toxicity is little.
Technical scheme of the present invention is as follows:
Improve the water miscible method of nano material, comprise the steps:
S10, nano particle is dissolved in organic solvent, makes solution A;
S20, in solution A, add the derivative solution of graphene oxide, and mix to obtain solution B;
S30, the aqueous phase layer in solution B is carried out after centrifugation, gained solid water cleans post-drying and makes the nano material after water-soluble improvement.
The invention still further relates to by described method and improve the nano material after water-soluble.
By the water miscible method of nano material of improving of the present invention, improve the nano material after water-soluble, have good water-soluble and multi-functional, polar solvent with and biological buffer in be not easy to reunite, and toxicity is lower, therefore can not produce harm to organism.
Accompanying drawing explanation
Fig. 1 (a), Fig. 1 (b) is the picture that the water miscible method of nano material is improved nano material after the water-soluble dissolving situation in redistilled water that improves by embodiment 1, this figure is the picture under the irradiation of 980nm laser apparatus, wherein Fig. 1 (a) is the photo under light field, Fig. 1 (b) is the photo under details in a play not acted out on stage, but told through dialogues, from Fig. 1 (a), can find out, method by embodiment 1 is improved up-conversion nanoparticles after water-soluble and in redistilled water, is had good water-soluble, there is no agglomeration, from Fig. 1 (b), can find out, the up-conversion nanoparticles that method by embodiment 1 is improved after water-soluble is still retaining fluorescence property,
Fig. 1 (c), Fig. 1 (d) is for improving nano material after water-soluble at the picture of the dissolving situation of phosphate buffered saline buffer (PBS) by the water miscible method of nano material of improving of embodiment 1, this figure is the picture under the irradiation of 980nm laser apparatus, wherein Fig. 1 (c) is the photo under light field, Fig. 1 (d) is the photo under details in a play not acted out on stage, but told through dialogues, from Fig. 1 (c), can find out, the up-conversion nanoparticles that method by embodiment 1 is improved after water-soluble has good dispersiveness in biological buffer, there is no agglomeration, from Fig. 1 (d), can find out, the up-conversion nanoparticles that method by embodiment 1 is improved after water-soluble is still retaining fluorescence property,
Fig. 2 (a), Fig. 2 (b) is the picture that the water miscible method of nano material is improved nano material after the water-soluble dissolving situation in redistilled water that improves in embodiment 3, Fig. 2 (a) is the photo under light field, from Fig. 2 (a), can find out, method by embodiment 1 is improved up-conversion nanoparticles after water-soluble and in redistilled water, is had good water-soluble, Fig. 2 (b) has put into the photo under light field in magnet situation in container, owing to improving water miscible nano material by magnet adsorption, therefore solution presents water white transparency shape, from Fig. 2 (b), can find out by of the present invention and improve the nano material that the water miscible method of nano material improves water-soluble and there is magnetic,
Fig. 2 (c), Fig. 2 (d) is the picture that the water miscible method of nano material is improved nano material after the water-soluble dissolving situation in phosphate buffered saline buffer (PBS) that improves in embodiment 3, Fig. 2 (c) is the photo under light field, from Fig. 2 (c), can find out, the up-conversion nanoparticles that method by embodiment 1 is improved after water-soluble has good dispersiveness in biological buffer, Fig. 2 (d) has put into the photo under light field in magnet situation in container, owing to improving water miscible nano material by magnet adsorption, therefore solution presents water white transparency shape, from Fig. 2 (d), can find out by of the present invention and improve the nano material that the water miscible method of nano material improves water-soluble and there is magnetic,
Fig. 3 (a), Fig. 3 (b) is the picture that the water miscible method of nano material is improved nano material after the water-soluble dissolving situation in redistilled water that improves in embodiment 4, Fig. 3 (a) is the photo under light field in 980nm laser illumination situation, from Fig. 3 (a), can find out that the present invention improves the water miscible method of nano material and improves nano material water-soluble and in redistilled water, have good water-soluble, there is no agglomeration, Fig. 3 (b) is in 980nm laser illumination situation, and in container, added the details in a play not acted out on stage, but told through dialogues photo in magnet situation, from then on figure can find out by of the present invention and improves the nano material that the water miscible method of nano material improves after water-soluble and have magnetic, fluorescence property,
Fig. 3 (c), Fig. 3 (d) is the picture that the water miscible method of nano material is improved nano material after the water-soluble dissolving situation in phosphate buffered saline buffer (PBS) that improves in embodiment 4, Fig. 3 (c) is the photo under light field in 980nm laser illumination situation, from Fig. 3 (c), can find out that the present invention improves the nano material that the water miscible method of nano material improves water-soluble and in biological buffer, has good dispersiveness, there is no agglomeration, Fig. 3 (d) is in 980nm laser illumination situation, and in container, added the details in a play not acted out on stage, but told through dialogues photo in magnet situation, from then on figure can find out by of the present invention and improves the nano material that the water miscible method of nano material improves after water-soluble and have magnetic, fluorescence property,
Fig. 4 improves the fluorescence property curve that the water miscible method of nano material is improved the up-conversion fluorescence nanoparticle after water-soluble in embodiment 1, wherein X-coordinate is wavelength, ordinate zou is fluorescence intensity, below line be by the method in embodiment 1, to improve the curve of the nano material of nano material after water-soluble, above line be the curve that improves the up-conversion fluorescence nanoparticle before water-soluble in embodiment 1, it is as can be seen from the figure, of the present invention that to improve the water miscible method of nano material relatively low to the fluorescent quenching rate of nano material;
GO-Fe in Fig. 5
3o
4line is in embodiment 3, to improve the magnetic property curve that the water miscible method of nano material is improved the nano material after water-soluble, Fe
3o
4line is not improve water miscible Fe
3o
4the magnetic property curve of nano material, wherein X-coordinate is magneticstrength, ordinate zou is magnetic torque; As can be seen from the figure, the water miscible method of nano material of improving of the present invention still can retain Fe
3o
4the superparamagnetic performance of nano particle;
Fig. 6 is the Cytotoxic curve that the water miscible method of nano material is improved the nano material obtaining after water-soluble that improves characterizing in embodiment 1 in embodiment 3, wherein ordinate zou is cell survival rate, as can be seen from the figure, the survival rate of the cell when concentration 2 μ g/ml and 10 μ g/ml of the nano material after the present embodiment resulting improvement is water-soluble is all higher, therefore, cytotoxicity is all lower.In figure, GO represents graphene oxide material, f-GO representative is with containing amino organic molecule or containing amino polymkeric substance or contain the graphene oxide that amino biomolecules is modified, it is the derivative of graphene oxide, GO-UCNPs represents the mixture of graphite oxide ene derivative and up-conversion nano material, the cytotoxicity of three kinds of materials is all lower, illustrates and take Graphene as basic material has good biocompatibility, at biological field, has good application prospect.
Embodiment
Referring to Fig. 7, a kind of water miscible method of nano material of improving, comprises the steps:
S10, nano particle is dissolved in organic solvent, makes solution A;
S20, in solution A, add the derivative solution of graphene oxide, and mix to obtain solution B;
S30, the aqueous phase layer in solution B is carried out after centrifugation, gained solid water cleans post-drying and makes the nano material after water-soluble improvement.
By the nano material tool improving after the water miscible method of nano material is improved of the present invention, have the following advantages:
(1) method provided by the present invention simply, effectively, is easily gone, by simple ultrasonic with stir, can obtain water-soluble extraordinary multifunctional nanocomposites.And the multifunctional nanocomposites obtaining has good dispersiveness in having the multiple solution of biocompatibility and damping fluid.
(2) multifunctional nanocomposites obtaining has lower toxicity, therefore can not produce harm to organism.
(3) with the present invention, various function nano materials can be loaded to the derivative surface of graphene oxide simultaneously, obtain thering is multifunctional nano composite material.
(4) use the derivative of graphene oxide as the carrier of phase transition, its useful load amount maximum can reach 1600%.
(5) after nano material being transferred to water by method of the present invention, under identical condition, the performance of nano material self is still retained.
(6) it is low that the multifunctional nanocomposites that uses method of the present invention to prepare has good wetting ability, multifunctionality and cytotoxicity, overcome the nanoparticle shortcomings such as wetting ability is poor aspect biocompatibility, function is few, cytotoxicity is large.Therefore in fields such as biomarker, biological detection, bio-imaging and disease treatments, there iing potential widespread use.
Preferably, the derivative of described graphene oxide is under the katalysis of 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride, graphene oxide and the graphite oxide ene derivative that contains amino organic molecule or contain amino polymkeric substance or contain amino biomolecular reaction generation.
Preferably, for water-soluble better improvement that can be to nano particle, the mass ratio of nano particle and graphite oxide ene derivative is 1:(0.06-10).
Preferably, in order to make nano particle better be dissolved in organic solvent, described organic solvent is cyclohexane or chloroform.
Preferably, in order to make nano particle better be dissolved in organic solvent, the mass volume ratio g/l of the usage quantity of nano particle and organic solvent in step S10 (mass unit is g, and volume unit is for rising) is (0.1-3): 1.
Preferably, described nano material is up-conversion fluorescence nanoparticle or ferriferrous oxide nano-particle.
Preferably, in order to make nano particle better be dissolved in organic solvent, the described method that nano particle is dissolved in to organic solvent is for to be placed in organic solvent by nano particle, and supersound process makes nano particle dissolve for 5 minutes-30 minutes.
Preferably, for graphene oxide solution can better be mixed with solution A, the blending means described in step S20 is with shaker concussion or with mixing under whipping appts agitation condition, mixing time is 40 seconds-480 seconds.
Preferably, in order to make the nano material after water-soluble improvement can be better separated from aqueous phase layer, the rotating speed of the whizzer of centrifugation described in step S30 be 14800 revs/min-20000 revs/min.
The invention still further relates to by described method and improve the nano material after water-soluble.
The derivative of graphene oxide of the present invention can be adopted preparation with the following method, can certainly adopt other method preparation of not mentioning in the present invention:
What the graphene oxide solution that is 1mg/mL by 10mL concentration and 10mL concentration were 10mg/mL contains in amino molecule, polymkeric substance or the biomolecule solution flask as for 50mL, ultrasonic 10 minutes.Taking afterwards 20mgEDC[1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride] solid joins in above-mentioned system, and ultrasonic 60 minutes.Separately take 280mgEDC ［ 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride ］ solid and join in above-mentioned system, stirring reaction 24 hours.After question response finishes, the derivative of graphene oxide is out centrifugal, and water cleaning is for several times, is finally distributed in water, is placed in 4 ℃ of environment and preserves, stand-by.
Up-conversion fluorescence nanoparticle of the present invention can adopt the preparation of one of following two kinds of methods:
(1) adopting oleic acid (Oleic acid) and octadecylene (Octadecylene) is solvent, and Rare Earths salt is that reactant carries out pyrolytic reaction:
Take YCl
3xH
2o, YbCl
3xH
2o and ErCl
3xH
2o is 1mmol(YCl altogether
3xH
2o, YbCl
3xH
2o and ErCl
3xH
2the mol ratio of O is 80:18:2 or 78:20:2), and add in 2mL methyl alcohol ultrasonic dissolution.Separately 6mL oleic acid and 15mL octadecylene are mixed in 50mL flask, above-mentioned methanol solution is poured in time mixed solution, be heated to 125 ℃ and stir, after making its dissolving and forming the solution of homogeneous transparent, be cooled to room temperature.By 2.5mmol NaOH and 4mmolNH
4f is dissolved in 6mL methyl alcohol, and ultrasonic dissolution slowly splashes in above-mentioned system with constant pressure funnel.After adding, by flask, as for heating 60min in the heating jacket of 125 ℃, object is by methyl alcohol volatilization complete (this step is extremely important, and can whether completely methyl alcohol volatilization affects reaction final product luminous).After treating methyl alcohol volatilization completely, insert prolong, remove air, logical water of condensation and argon gas, also stir constant temperature to 300 ℃ left and right, and the reaction times is 1h.After question response end temp declines, the particle in system is out centrifugal and use ethanol or water to clean for several times, dry, collect powder standby.
(2) adopting oleic acid (oleic acid) and ethanol (ethanol) is solvent, and rare earth nitrate is that reactant carries out hydro-thermal reaction:
Pipette Y (NO
3)
3xH
2o, Yb (NO
3)
3xH
2o, Er (NO
3)
3xH
2o and MnCl
21mmol(Y (NO altogether
3)
3xH
2o, Yb (NO
3)
3xH
2o, Er (NO
3)
3xH
2o and MnCl
2mol ratio be 40:18:2:30 or 38:20:2:30), cumulative volume is 5mL, stirs.Afterwards this mixing solutions is joined stirred contain 0.3000g sodium hydroxide, 1.5mL intermediate water, in the mixed system of 5mL ethanol and 5mL oleic acid, stir after 30min, add wherein the 2mL NaF aqueous solution (2mol/L), after stirring, they are transferred in tetrafluoroethylene reactor, be warming up to 200 ℃ of temperature, reaction 6h.After question response end temp declines, the particle in system is out centrifugal and use ethanol or water to clean for several times, dry, collect powder standby.
Ferroferric oxide magnetic nano-particles of the present invention can be adopted preparation with the following method:
Adopting oleic acid and oleyl amine is solvent, ferric acetyl acetonade (Fe (acac)
3) be the former ferroferric oxide nano granules of preparing of iron:
Take 0.5060g Fe (acac)
3be dissolved in 20mL dehydrated alcohol stirring and dissolving.Separately get 6mL oleic acid and 6mL oleyl amine and be mixed in above-mentioned system, continue to stir 30min.Transfer to afterwards in 45mL tetrafluoroethylene reactor, be warming up to 220 ℃, react 6 hours.After question response end temp declines, the particle in system is out centrifugal and use second alcohol and water to clean for several times, dry, collect powder standby.
Up-conversion fluorescence nanoparticle and ferroferric oxide magnetic nano-particles take below as example, provide several specific embodiments, the present invention is equally applicable to the phase transition of other nano material except up-conversion fluorescence nanoparticle and ferroferric oxide magnetic nano-particles, and water-soluble, lower toxicity and the multifunctionality that after phase transition, can make equally multifunctional nano composite material obtain.
Take up-conversion fluorescence nanoparticle 1mg, join in 1mL chloroform, make up-conversion fluorescence nano-particle solution.Then supersound process 10 minutes, until up-conversion fluorescence nanoparticle is dissolved in described organic solvent completely, adds the derivative solution of 1mL graphene oxide, and concentration is 0.2mg/ml.Then described solution is placed on vibrator and is shaken 1 minute.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 14800 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has fluorescence property and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
Take up-conversion fluorescence nanoparticle 3mg, join in 1mL hexanaphthene, make up-conversion fluorescence nano-particle solution.Then supersound process 10 minutes, until up-conversion fluorescence nanoparticle is dissolved in described organic solvent completely, adds the derivative solution of 1mL graphene oxide, and concentration is 0.18mg/ml.Then described solution is placed on vibrator and is shaken 1 minute.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 14800 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has fluorescence property and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
Embodiment 3
Take ferroferric oxide magnetic nano-particles 0.8mg, join in 1mL chloroform, make ferriferrous oxide nano-particle solution.Then supersound process 10 minutes, until ferroferric oxide magnetic nano-particles is dissolved in described organic solvent completely, adds the derivative solution of 1mL graphene oxide, and concentration is 0.2mg/ml.Then described solution is placed on vibrator and is shaken 1 minute.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 14800 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has superparamagnetic performance and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
Embodiment 4
Take ferroferric oxide magnetic nano-particles 0.5mg, up-conversion nanoparticles 0.5mg, joins in 1mL chloroform, makes mix nanoparticles solution.Then supersound process 10 minutes, until ferroferric oxide magnetic nano-particles and upper conversion nano fluorescent nano particles are dissolved in described organic solvent completely, adds the derivative solution of 1mL graphene oxide, and concentration is 0.3mg/ml.Then described solution is placed on vibrator and is shaken 1 minute.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 14800 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has fluorescence property, superparamagnetic performance and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
Embodiment 5
Take ferroferric oxide magnetic nano-particles 1mg, join in 10mL chloroform, make mix nanoparticles solution.Then supersound process 30 minutes, until ferroferric oxide magnetic nano-particles and upper conversion nano fluorescent nano particles are dissolved in described organic solvent completely, adds the derivative solution of 1mL graphene oxide, and concentration is 0.1mg/ml.Then described solution is placed on vibrator and is shaken 40 seconds.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 14800 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has fluorescence property, superparamagnetic performance and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
Embodiment 6
Take up-conversion nanoparticles 0.5mg, join 1mL chloroform, make mix nanoparticles solution.Then supersound process 5 minutes, until ferroferric oxide magnetic nano-particles and upper conversion nano fluorescent nano particles are dissolved in described organic solvent completely, adds the derivative solution of 20mL graphene oxide, and concentration is 0.25mg/ml.Then described solution is placed on vibrator and is shaken 8 minutes.After concussion finishes, isolate aqueous phase layer.By the solution of aqueous phase layer centrifugal treating under the rotating speed of 20000 revs/min of centrifuge speeds, post-drying of washed with de-ionized water for the multifunctional nanocomposites obtaining after centrifugal treating, collects powder.This multifunctional nanocomposites has fluorescence property, superparamagnetic performance and good water-soluble, and has lower toxicity, therefore can not produce harm to organism.
The sequencing of above embodiment only, for ease of describing, does not represent the quality of embodiment.
Finally it should be noted that: above embodiment only, in order to technical scheme of the present invention to be described, is not intended to limit; Although the present invention is had been described in detail with reference to previous embodiment, those of ordinary skill in the art is to be understood that: its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
1. improve the water miscible method of nano material, it is characterized in that, comprise the steps:
S10, nano particle is dissolved in organic solvent, makes solution A;
S20, in solution A, add the derivative solution of graphene oxide, and mix to obtain solution B;
S30, the aqueous phase layer in solution B is carried out after centrifugation, gained solid water cleans post-drying and makes the multi-functional nanometer material after water-soluble improvement.
2. the water miscible method of nano material of improving according to claim 1, it is characterized in that, the derivative of described graphene oxide is under the katalysis of 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride, graphene oxide and the graphite oxide ene derivative that contains amino organic molecule or contain amino polymkeric substance or contain amino biomolecular reaction generation.
3. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, the mass ratio of nano particle and graphite oxide ene derivative is 1:(0.06-10).
4. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, described organic solvent is hexanaphthene or chloroform.
5. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, in step S10, the mass volume ratio g/l of the usage quantity of nano particle and organic solvent is (0.1-3): 1.
6. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, described nano material is up-conversion fluorescence nanoparticle or ferriferrous oxide nano-particle.
7. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, the described method that nano particle is dissolved in to organic solvent is for to be placed in organic solvent by nano particle, and supersound process makes nano particle dissolve for 5 minutes-30 minutes.
8. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, the blending means described in step S20 is with shaker concussion or with mixing under whipping appts agitation condition, mixing time is 40 seconds-480 seconds.
9. the water miscible method of nano material of improving according to claim 1 and 2, is characterized in that, the rotating speed of the whizzer of centrifugation described in step S30 is 14800 revs/min-20000 revs/min.
10. one kind is improved the nano material after water-soluble by method described in claim 1-9 any one.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371714A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Molybdenum trioxide-graphene oxide composite material and preparation method thereof |
| CN105733586A (en) * | 2016-04-27 | 2016-07-06 | 武汉理工大学 | Method for preparing AREF4:Ln<3+> up-conversion microcrystals by combining thermal decomposition method with hydrothermal method |
| CN109250773A (en) * | 2018-10-30 | 2019-01-22 | 李忠 | A kind of sewage treatment composite nano materials and preparation method thereof |
| CN109796585A (en) * | 2019-01-30 | 2019-05-24 | 陕西科技大学 | A method of using the water-soluble nano material of three arm cross-linking methods preparation green light |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780420A (en) * | 2010-03-05 | 2010-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of metal and graphene composite catalyst |
| CN101913600A (en) * | 2010-08-27 | 2010-12-15 | 上海交通大学 | Method for preparing graphene/semiconductor quantum dot composite material |
| CN102500287A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Graphene/modified titanium dioxide nano sol composite material and preparation method thereof |
| CN102671625A (en) * | 2012-05-02 | 2012-09-19 | 湖北富邦科技股份有限公司 | Method for preparing graphene magnetic nanometer composite materials |
| CN102674476A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Chemical preparation method of magnetic graphene |
-
2012
- 2012-09-21 CN CN201210357211.1A patent/CN103666446B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780420A (en) * | 2010-03-05 | 2010-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of metal and graphene composite catalyst |
| CN101913600A (en) * | 2010-08-27 | 2010-12-15 | 上海交通大学 | Method for preparing graphene/semiconductor quantum dot composite material |
| CN102500287A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Graphene/modified titanium dioxide nano sol composite material and preparation method thereof |
| CN102671625A (en) * | 2012-05-02 | 2012-09-19 | 湖北富邦科技股份有限公司 | Method for preparing graphene magnetic nanometer composite materials |
| CN102674476A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Chemical preparation method of magnetic graphene |
Non-Patent Citations (1)
| Title |
|---|
| 张燚，等: "Fe3O4磁性纳米粒子-氧化石墨烯复合材料的可控制备及结构与性能表征", 《物理化学学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371714A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Molybdenum trioxide-graphene oxide composite material and preparation method thereof |
| CN105733586A (en) * | 2016-04-27 | 2016-07-06 | 武汉理工大学 | Method for preparing AREF4:Ln<3+> up-conversion microcrystals by combining thermal decomposition method with hydrothermal method |
| CN105733586B (en) * | 2016-04-27 | 2018-09-11 | 武汉理工大学 | A kind of thermal decomposition-hydro-thermal combination preparation AREF4:Ln3+The preparation method of upper conversion micron crystalline substance |
| CN109250773A (en) * | 2018-10-30 | 2019-01-22 | 李忠 | A kind of sewage treatment composite nano materials and preparation method thereof |
| CN109796585A (en) * | 2019-01-30 | 2019-05-24 | 陕西科技大学 | A method of using the water-soluble nano material of three arm cross-linking methods preparation green light |
| CN109796585B (en) * | 2019-01-30 | 2021-01-26 | 陕西科技大学 | Method for preparing green light-emitting water-soluble nano material by adopting three-arm cross-linking method |
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