CN102240532A - Method for preparing inorganic nano particle/silicon dioxide composite microspheres with core shell structure - Google Patents
Method for preparing inorganic nano particle/silicon dioxide composite microspheres with core shell structure Download PDFInfo
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Abstract
The invention relates to a method for preparing inorganic nano particle/silicon dioxide composite microspheres with a core shell structure, comprising the following steps of: dispersing inorganic nano particles into a nonpolar organic solvent, and adding hydrophilic macromolecules as a stabilizer; adding a reactant to a polar reaction medium, such as ethanol and the like, and ultrasonically and uniformly stirring, wherein the volume ratio of the nonpolar organic solvent to the polar reaction medium is 1:5-1:20; adding ethyl orthosilicate and ammonia to a reaction system, wherein the mass ratio of the inorganic nano particles to the ethyl orthosilicate is 1:100-1:10, and the volume ratio of the ammonia to the ethyl orthosilicate is1:10-1:1; and preparing the composite microspheres with the average grain diameter of 15-600 nm. The invention has the advantages that a silicon dioxide shell layer can be prepared in a polar organic solvent through the oil-soluble inorganic nano particles, and therefore, not only the formation of the silicon dioxide shell layer is well controlled and promoted, but also a complex isolation and purification process in an experiment process is simplified; and all reactions are carried out in one system, and therefore an experiment is simple and efficient.
Description
Technical field
The present invention relates to a kind of composite that can be applicable to biomedical sector, especially relate to a kind of method for preparing nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
Background technology
Recent two decades comes, and big quantity research has reported that some nano particles can be used to biosystem.Particularly, the magnetic nanometer and the quantum dot of the superparamagnetism that employing high temperature oil phase legal system is equipped with, because its potential biologic applications is worth, attract a lot of researchers' concern, can be widely used in targeted therapy, fluorescence imaging and the biology sensor etc. of magnetic resonance imaging (MRI), medicine.Inorganic nano-particle has been obtained development rapidly aspect biologic applications.
But, because inorganic nano-particle contains heavy metal element, for example, cobalt, chromium, manganese, iron, therefore, they have cytotoxicity, also make inorganic nano-particle be subjected to certain restriction aspect biologic applications.According to the literature, forming the dissolving that shell can prevent poisonous element with the amorphous silicon of biologically inert parcel inorganic nano-particle and reveal, is a method effectively to the chemical stability that reduces cytotoxic effect and be increased in the aqueous solution.In addition, SiO
2The Si-OH group on surface can be easy to be modified, and makes inorganic nano-particle become easy in biologic applications.
The inorganic nano-particle that adopts high temperature oil phase legal system to be equipped with is an oil-soluble, generally can be dispersed in well in the nonpolar organic solvent, and for example, chloroform, cyclohexane, toluene can not be dispersed in water and the ethanol.But, can better controlled SiO in ethanol
2Forming process because this restriction, make and directly use SiO
2It is difficult that the coated inorganic nano particle becomes.Therefore, bibliographical information is arranged some be nuclear with the inorganic nano-particle, silica is the preparation method of the complex microsphere of shell (NPSiO2).Adopt (TEOS) a series of hydrolysis and the condensation reaction of organo-silicon compound, surfactant or hydrophilic macromolecule and ethyl orthosilicate that the inorganic nano-particle sub-surface is carried out modification.But these all methods have all related to loaded down with trivial details surface modification and purge process.
Summary of the invention
Purpose of the present invention aims to provide a kind of method for preparing nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere simply, efficiently, emphasis has solved this problem of synthetic silica shell in ethanol isopolarity reaction medium, particle good dispersion in course of reaction does not have precipitation or agglomeration.The average grain diameter of the inorganic nano-particle/SiO 2 composite microsphere with nucleocapsid structure of preparation is 15～600nm, and particle diameter is even, nucleocapsid structure is obvious, and inorganic nano-particle is coated fully to be entered in the silica shell, has expanded the application of inorganic nano-particle at biomedical sector.
The preparation method of nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere of the present invention may further comprise the steps:
1) inorganic nano-particle is dispersed in the non-polar organic solvent, adds hydrophilic macromolecule as stabilizing agent; The mass ratio of inorganic nano-particle and hydrophilic macromolecule is 1: 5～1: 200;
2) reactant with step 1) joins in the ethanol isopolarity reaction medium, and is ultrasonic, stirs; The volume ratio of non-polar organic solvent and polar reaction medium is 1: 5～1: 20;
3) to step 2) reaction system in add ethyl orthosilicate (TEOS) and ammoniacal liquor, inorganic nano-particle is 1: 100～1: 10 with the ratio of the quality of ethyl orthosilicate, ammoniacal liquor is 1: 10～1: 1 with the ratio of the volume of ethyl orthosilicate; Reaction 12～48h, centrifuge washing makes average grain diameter at 15～600nm, inorganic nano-particle/silicon dixoide nucleocapsid structure complex microsphere.
Described inorganic nano-particle is meant one or more the combination in metal nanoparticle, semiconductor nano particle or the magnetic nano-particle of average grain diameter between 1～100nm.
Described inorganic nano-particle is selected from Au, Ag, CdS, CdSe, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/ZnSe, CdTe/ZnS, CdTe/CdS, CdTe/ZnSe, CdSeTe or Fe
3O
4The combination of wherein one or more.
Described organic solvent is one or more the combination in chloroform, cyclohexane, the toluene.
Described hydrophilic macromolecule is one or more the combination in PEO (PEO), polymine (PEI) and the polyvinylpyrrolidone (PVP).
Described polar organic solvent is one or both the combination in ethanol, the acetonitrile.
Our method can overcome some problems of above-mentioned existence.When having hydrophilic macromolecule PEO (PEO), polymine (PEI) and polyvinylpyrrolidone (PVP), because hydrophilic macromolecule makes inorganic nano-particle can not form large-sized reunion or precipitation in ethanol isopolarity organic solvent to the surface-stable effect of having played of inorganic nano-particle.This surface-stable effect makes to be coated with high molecular inorganic nano-particle and to can be good at being dispersed in the ethanol isopolarity organic solvent.Because hydrophilic macromolecule has stabilizer function, and can impel the inorganic nano-particle sub-surface to adsorb unbodied silicon, therefore, can form the silicon shell in the inorganic nano-particle sub-surface that has hydrophilic macromolecule to coat.The advantage of this method is that process is simple, and institute responds all in an individual system, does not need loaded down with trivial details isolation and purge process.
The present invention compared with prior art is characterised in that, adopt hydrophilic macromolecule as intermediate medium, not only make inorganic nano-particle in polar organic solvent, can be good at disperseing, and can control and promote inorganic nano-particle absorption silicon, help forming silica shell.
Advantage of the present invention mainly is, oil-soluble inorganic nano-particle can prepare silica shell in polar organic solvent, not only can better controlled and promote the formation of silica shell, and isolation and purge process loaded down with trivial details in the experimentation have been simplified, institute responds and all carries out in an individual system, makes experiment simple efficient.
Description of drawings
Nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere macrograph described in Fig. 1: the embodiment 1.
The fluorescence spectrum of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere that makes among Fig. 2: the embodiment 2.
The magnetic responsiveness curve of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere that makes among Fig. 3: the embodiment 4.
The fluorescence spectrum of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere that makes among Fig. 4: the embodiment 6.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are made detailed description: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, and given detailed embodiment and process are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1:
Step 1, taking by weighing the 2mg emission wavelength is the CdSeTe quantum dot of 517nm, and quantum dot is dissolved in the 0.5ml chloroform, adding 10mgPVP is a stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in the 10ml ethanol, and it is even to be stirred to system;
Step 3 adds 30 μ l ethyl orthosilicates (TEOS) and 15 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 12h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
Fig. 1 is the macrograph of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere of preparation, as shown in the figure, the inorganic nano-particle of preparation/silicon dixoide nucleocapsid structure complex microsphere particle diameter is even, favorable dispersibility, no agglomeration, nucleocapsid structure is clear, complete.
Embodiment 2:
Step 1, taking by weighing the 1mg emission wavelength is the CdSe/ZnS quantum dot of 564nm, and quantum dot is dissolved in the 1ml chloroform, adding 200mgPEI is a stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in the 10ml acetonitrile, and it is even to be stirred to system;
Step 3 adds 10 μ l ethyl orthosilicates (TEOS) and 10 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 36h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.Fig. 2 is the fluorescence spectrum of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere of preparation, and as shown in Figure 2, fluorescent emission peak-to-peak type is good, and half-peak breadth is narrower.
Embodiment 3:
Step 1, taking by weighing the 4mg emission wavelength is the CdSe quantum dot of 650nm, and quantum dot is dissolved in the 2ml cyclohexane, adding 200mgPEO is a stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in 5ml acetonitrile and the 5ml ethanol, and it is even to be stirred to system;
Step 3 adds 60 μ l ethyl orthosilicates (TEOS) and 10 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.
Embodiment 4:
Step 1 takes by weighing 2mg magnetic nano-particle Fe
3O
4, magnetic nano-particle is dissolved in the 1ml toluene, adding 50mgPEI and 50mgPVP is stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in 5ml acetonitrile and the 5ml ethanol, and it is even to be stirred to system;
Step 3 adds 200 μ l ethyl orthosilicates (TEOS) and 20 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.Fig. 3 is the magnetic responsiveness curve of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere ball of preparation, and as shown in the figure, the magnetic response curve is good.
Embodiment 5:
Step 1 takes by weighing the 3mgAu nano particle, and the Au nano particle is dissolved in 0.5ml toluene and the 1ml chloroform, and adding 20mgPEI, 20mgPVP and 20mgPEO is stabilizing agent;
Step 2 joins the reactant of step 1 in 10ml acetonitrile and the 5ml ethanol, and it is even to be stirred to system;
Step 3 adds 50 μ l ethyl orthosilicates (TEOS) and 10 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.
Embodiment 6:
Step 1, taking by weighing the 0.5mg emission wavelength is the CdTe/CdS quantum dot of 564nm and the CdS quantum dot that the 0.5mg emission wavelength is 650nm, and quantum dot is dissolved in the 2ml chloroform, adding 150mgPEO is a stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in 10ml acetonitrile and the 5ml ethanol, and it is even to be stirred to system;
Step 3 adds 80 μ l ethyl orthosilicates (TEOS) and 20 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.Fig. 4 is the fluorescence spectrum of the nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere of preparation, and as shown in the figure, fluorescent emission peak-to-peak type is good, and half-peak breadth is narrower, and bimodal energy is separated.
Embodiment 7:
Step 1 takes by weighing 1mg magnetic nano-particle Fe
3O
4With the 1mgCdSe/ZnSe quantum dot, magnetic nano-particle and quantum dot are dissolved in 1ml toluene and the 1ml chloroform, adding 50mgPEO and 50mgPVP is stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in 5ml acetonitrile and the 10ml ethanol, and it is even to be stirred to system;
Step 3 adds 100 μ l ethyl orthosilicates (TEOS) and 30 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.
Embodiment 8:
Step 1 takes by weighing 1mgAu nano particle and 1mg CdTe/CdS quantum dot, and Au nano particle and quantum dot are dissolved in 1ml cyclohexane and the 1ml chloroform, and adding 50mgPEO and 50mgPEI is stabilizing agent, ultrasonic being uniformly dispersed;
Step 2 joins the reactant of step 1 in 10ml acetonitrile and the 5ml ethanol, and it is even to be stirred to system;
Step 3 adds 80 μ l ethyl orthosilicates (TEOS) and 30 μ l ammoniacal liquor in the reaction system of step 2, mixing speed is 3000r/min, reaction 48h, and centrifuge washing makes nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere.
The complex microsphere particle diameter of preparation is even, favorable dispersibility, and no agglomeration, nucleocapsid structure is clear, complete.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. the preparation method of nucleocapsid structure inorganic nano-particle/SiO 2 composite microsphere is characterized in that step is as follows:
1) inorganic nano-particle is dispersed in the non-polar organic solvent, adds hydrophilic macromolecule as stabilizing agent; The mass ratio of inorganic nano-particle and hydrophilic macromolecule is 1: 5～1: 200;
2) reactant with step 1) joins in the polar reaction medium, and is ultrasonic, stirs; The volume ratio of non-polar organic solvent and polar reaction medium is 1: 5～1: 20,
3) to step 2) reaction system in add ethyl orthosilicate and ammoniacal liquor, inorganic nano-particle is 1: 100～1: 10 with the ratio of the quality of ethyl orthosilicate, ammoniacal liquor is 1: 10～1: 1 with the ratio of the volume of ethyl orthosilicate; Reaction 12～48h, centrifuge washing makes average grain diameter at 15～600nm, inorganic nano-particle/silicon dixoide nucleocapsid structure complex microsphere.
2. preparation method as claimed in claim 1 is characterized in that described inorganic nano-particle, is meant one or more the combination in metal nanoparticle, semiconductor nano particle or the magnetic nano-particle of average grain diameter between 1～100nm.
3. preparation method as claimed in claim 2 is characterized in that described inorganic nano-particle is selected from Au, Ag, CdS, CdSe, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/ZnSe, CdTe/ZnS, CdTe/CdS, CdTe/ZnSe, CdSeTe or Fe
3O
4The combination of wherein one or more.
4. preparation method as claimed in claim 1 is characterized in that described organic solvent is one or more the combination in chloroform, cyclohexane, the toluene.
5. preparation method as claimed in claim 1 is characterized in that described hydrophilic macromolecule is one or more the combination in PEO, polymine or the polyvinylpyrrolidone.
6. preparation method as claimed in claim 1 is characterized in that described polar organic solvent is one or both the combination in ethanol, the acetonitrile.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102416468A (en) * | 2011-11-21 | 2012-04-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nano metal leaf and preparation method thereof |
| CN102671588A (en) * | 2012-05-15 | 2012-09-19 | 同济大学 | Method for synthetizing nano silver/silicon dioxide core-shell particles in water system |
| CN104211071A (en) * | 2014-09-05 | 2014-12-17 | 哈尔滨工业大学 | Synthetic method of CdS@SiO2 nano composite material |
| CN104259474A (en) * | 2014-09-23 | 2015-01-07 | 中国科学院化学研究所 | Preparation method of golden-core-shell structure nanometer material |
| CN104388077A (en) * | 2014-10-31 | 2015-03-04 | 中国科学院理化技术研究所 | Silicon dioxide-filled nano-cluster composite material and preparation method and application thereof |
| CN105670630A (en) * | 2016-02-23 | 2016-06-15 | 华中科技大学 | Water-soluble rare-earth-doped nanocrystals and preparation method and application thereof |
| CN105754603A (en) * | 2016-05-11 | 2016-07-13 | 青岛海信电器股份有限公司 | Quantum dot assembly as well as preparation method and application thereof |
| CN109986848A (en) * | 2017-12-29 | 2019-07-09 | 财团法人工业技术研究院 | Composite fabric |
| CN110293232A (en) * | 2018-03-23 | 2019-10-01 | 中国人民解放军军事科学院军事医学研究院 | A kind of method that ultrasonic wave added hydroxylamine hydrochloride seed mediated growth method prepares silicon core golden shell nano particle |
| WO2020150886A1 (en) * | 2019-01-22 | 2020-07-30 | 东莞东阳光科研发有限公司 | Polyimide microsphere slurry, composite separator, and lithium-ion battery |
| CN111929277A (en) * | 2020-06-03 | 2020-11-13 | 中国科学院苏州生物医学工程技术研究所 | One-dimensional assembly of noble metal nanoparticles with adjustable spacing and application of assembly in nano sensor |
| CN112563016A (en) * | 2020-12-23 | 2021-03-26 | 四川迈克生物新材料技术有限公司 | Preparation method of magnetic microspheres for nucleic acid extraction, prepared product and application |
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| CN102416468A (en) * | 2011-11-21 | 2012-04-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nano metal leaf and preparation method thereof |
| CN102416468B (en) * | 2011-11-21 | 2013-06-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nano metal leaf and preparation method thereof |
| CN102671588A (en) * | 2012-05-15 | 2012-09-19 | 同济大学 | Method for synthetizing nano silver/silicon dioxide core-shell particles in water system |
| CN104211071A (en) * | 2014-09-05 | 2014-12-17 | 哈尔滨工业大学 | Synthetic method of CdS@SiO2 nano composite material |
| CN104259474A (en) * | 2014-09-23 | 2015-01-07 | 中国科学院化学研究所 | Preparation method of golden-core-shell structure nanometer material |
| CN104388077A (en) * | 2014-10-31 | 2015-03-04 | 中国科学院理化技术研究所 | Silicon dioxide-filled nano-cluster composite material and preparation method and application thereof |
| CN105670630B (en) * | 2016-02-23 | 2019-06-18 | 华中科技大学 | A kind of water-solubility rare-earth dopen Nano crystal and its preparation method and application |
| CN105670630A (en) * | 2016-02-23 | 2016-06-15 | 华中科技大学 | Water-soluble rare-earth-doped nanocrystals and preparation method and application thereof |
| CN105754603A (en) * | 2016-05-11 | 2016-07-13 | 青岛海信电器股份有限公司 | Quantum dot assembly as well as preparation method and application thereof |
| CN109986848A (en) * | 2017-12-29 | 2019-07-09 | 财团法人工业技术研究院 | Composite fabric |
| CN110293232A (en) * | 2018-03-23 | 2019-10-01 | 中国人民解放军军事科学院军事医学研究院 | A kind of method that ultrasonic wave added hydroxylamine hydrochloride seed mediated growth method prepares silicon core golden shell nano particle |
| WO2020150886A1 (en) * | 2019-01-22 | 2020-07-30 | 东莞东阳光科研发有限公司 | Polyimide microsphere slurry, composite separator, and lithium-ion battery |
| CN113169418A (en) * | 2019-01-22 | 2021-07-23 | 东莞东阳光科研发有限公司 | Polyimide microsphere slurry, composite diaphragm and lithium ion battery |
| CN111929277A (en) * | 2020-06-03 | 2020-11-13 | 中国科学院苏州生物医学工程技术研究所 | One-dimensional assembly of noble metal nanoparticles with adjustable spacing and application of assembly in nano sensor |
| CN111929277B (en) * | 2020-06-03 | 2021-06-01 | 中国科学院苏州生物医学工程技术研究所 | One-dimensional assembly of noble metal nanoparticles with adjustable spacing and application of assembly in nano sensor |
| CN112563016A (en) * | 2020-12-23 | 2021-03-26 | 四川迈克生物新材料技术有限公司 | Preparation method of magnetic microspheres for nucleic acid extraction, prepared product and application |
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Application publication date: 20111116 |