CN105482806B - A kind of fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid and preparation method thereof - Google Patents
A kind of fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid and preparation method thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Abstract
Fluorescence mesoporous inorganic oxide nano-particle the invention discloses a kind of nucleocapsid and preparation method thereof.The fluorescence mesoporous inorganic oxide nano-particle of the present invention is nucleocapsid, and core is fine and close solid bead, is silica, iron oxide or manganese oxide inorganic nano-particle；Shell is the group modified meso-hole structure of organic fluorescence.The organic fluorescence group of the shell is organic fluorescence double end silicon source structure, and representation is (R ' O)3Si‑R‑Si(R’O)3, wherein R ' is C1‑C4Alkyl, R are fluorescent chromophore.The preparation that the present invention passes through 1) inorganic oxide nanoparticles；2) preparation of nucleocapsid oxide nano-particles；3) three step of removal of shell mesopore orbit template is prepared.The beneficial effects of the present invention are：Nano-particle has regular pattern and good monodispersity；Skeleton organic fluorescence group is modified, and fluorescence property is controllable；Reaction condition is mild, prepares simple, easily repetition.
Description
Technical field
The invention belongs to advanced technical field of nano material, and in particular to one kind has regular pattern and good monodispersity
New nucleocapsid fluorescence mesoporous inorganic oxide nano-particle and preparation method thereof.
Background technology
Fluorescence silica material due to characteristics such as its higher specific surface area, highlighted fluorescence, sensor, pharmaceutical indications with
And there is preferable application in the fields such as biology imaging.However, the fluorescence functional group of the fluorescent nano particles of the current overwhelming majority is all
It is that either the modes such as Graft Method are introduced among particle surface or duct by sedimentation, load method so that nanoparticle sub-aperture
The reduction of road utilization rate, while also easily dyestuff is caused to leak, the fluorescence property of particle is not only reduced, also limits them in life
The application development of object field particularly pharmaceutical carrier field.At the same time, with requiring fluorescent nano particles complex function
Higher and higher, the research of people's nucleocapsid fluorescent nano particles increasingly complex to structure is also increasingly paid attention to.By preparing nucleocapsid
A kind of performance is introduced into nuclear particle by structure nano particle, such as：Fluorescence or superparamagnetic etc., while introduced in shell
A kind of another kind performance, such as fluorogen, chelating agent etc., by cleverly spatial arrangement, are realized on a nano-particle
Multiple functions it is compound, provide the thinking of new approach for the Complex Function of nano-particle.
In current report, the report of the preparation of all kinds of core-shell structure nanometer particles has all kinds of organo-functional groups, such as
Alkene, alkynes and all kinds of organo-functional groups are introduced into the report gone in nano-particle shell, have material ultraviolet or visible
Light absorpting ability, and apply in fields such as separation, ion detection, removal and gas storages.However in the synthesis process, shell
Structure may reunite, wrap up the problems such as uneven so that the pattern and particle diameter distribution of the nano-particle of preparation are difficult to control
System, restricts the further application and development of such material.Therefore how to obtain possessing regular appearance, the shell bone of size tunable
The modified nucleocapsid fluorescence silicon oxide nanoparticle of frame organic fluorescence group is still a huge challenge.
The content of the invention
It is a kind of with regular pattern and single point good it is an object of the invention to propose for overcome the deficiencies in the prior art
Dissipate fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid of property and preparation method thereof.
The present invention, by one kettle way, fluorogen is introduced using the mode of copolycondensation using different compact nanometer particles as core
It is glimmering so as to be prepared for the modified nucleocapsid of shell skeleton organic fluorescence group into the shell inorganic skeleton of nucleocapsid silicon oxide nanoparticle
Light mesoporous silicon dioxide nano particle.The fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid proposed by the present invention, tool
There are regular pattern and good monodispersity, be the functional nano material that a kind of shell skeleton organic fluorescence group is modified, duct is unimpeded
Material.Phase introduces fluorescence functional group in preparation process middle skeleton so that nano-particle has preferable light absorpting ability and fluorescence
Performance；After removing template by extraction simultaneously, the duct of nano-particle is completely unimpeded, and becoming a kind of has well loaded energy
The carrier material of power.At the same time, due to the compact nanometer particle that core uses for selection, it is more to impart core-shell nano
Performance so that such material is expected to have good potential application foreground in fields such as biology imaging, separation.
The present invention provides a kind of fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid, is nucleocapsid, core is
Fine and close solid bead, in silica, iron oxide or manganese oxide inorganic nano-particle any one；Shell is organic fluorescence base
The modified meso-hole structure of group.
In the present invention, the organic fluorescence group of the shell is organic fluorescence double end silicon source structure, and the organic fluorescence is double
Head silicon source representation is (R ' O)3Si-R-Si(R’O)3, wherein R ' is C1-C4Alkyl, R are fluorescent chromophore.Preferably, institute
It is the fluorescent chromophore containing aromatic rings to state the R in organic fluorescence double end silicon source structure.It is further preferred that the R be containing
Biphenyl, anthracene, naphthalene or in appoint one or more aromatic rings fluorescent chromophore.
In the present invention, the meso-hole structure of shell is to include various tubulose ducts, the meso-hole structure in spherical duct.Pore passage structure
It is p6mm in space group,P63/ mmc,One of which is several
Mixing.
It is specific to walk the present invention also provides a kind of preparation method of the fluorescence mesoporous inorganic oxide nano-particle of nucleocapsid
It is rapid as follows：
(1) preparation of inorganic oxide nanoparticles
The inorganic oxide nanoparticles are dense oxide silicon, compact iron oxide or dense oxide manganese inorganic nano-particle
Son；
(2) preparation of core-shell structure copolymer oxide nano-particles
The inorganic oxide nanoparticles of step (1) are suspended in absolute ethyl alcohol and the mixed solution of secondary water first,
Adjusting PH with base is added in after ultrasonic disperse, the mixed liquor for being subsequently added into the template prepared in advance, absolute ethyl alcohol and secondary water continues
Stirring, then inorganic silicon source and the compound reaction containing organic fluorescent chromophore are added in into reaction solution；Finally by reacting liquid filtering,
Upper strata core-shell particles washing is dried in vacuo at room temperature, is ground；Wherein：The compound containing organic fluorescent chromophore is organic
Fluorescence double end silicon source structure, representation are (R ' O)3Si-R-Si(R’O)3, wherein R ' is C1-C4Alkyl, R are fluorescence color development
Group；
(3) removal of shell mesopore orbit template
The core-shell structure copolymer oxide nano-particles that step (2) obtains are suspended in ethyl alcohol, ammonium acetate is then added in, this is mixed
Close solution be heated to flowing back, when 1-2 is small after, reaction solution is cooled to room temperature, and is filtered, is washed, particle room temperature in vacuo drying, obtain core
The fluorescence mesoporous inorganic oxide nano-particle of shell structure.
In above-mentioned steps (1), when inorganic oxide nanoparticles are dense oxide silicon nanos, by the following method
It is prepared：
Alkali is added to together with inorganic silicon source in alkylol, and when reaction 10~24 is small, by reaction solution centrifuge washing, use is anhydrous
Respectively washing for several times, collects product cake for ethyl alcohol and secondary water, and is dried in vacuo at room temperature, obtains target nano-particle；It is alkali, inorganic
The volume ratio that feeds intake (2.56~100) of silicon source and alkylol:(1.42~200):(33~3000)；
When the inorganic oxide nanoparticles are dense oxide Fe nanometer particles, it is prepared via a method which to obtain：
By FeCl3, citric acid, sodium acetate, be added in alkylol, be transferred to water heating kettle after stirring, 200~300 DEG C are anti-
Answer 10~24 it is small when, be cooled to room temperature, after obtained black nano particle is washed for several times with absolute ethyl alcohol and deionized water, disperse
In ethyl alcohol；Wherein：FeCl3, citric acid and sodium acetate mass ratio be (85~2000):(48~3000):(1.75~
500)；FeCl3Mass volume ratio with alkylol is (85~2000)：(300~40000) mg/mL.
In above-mentioned steps (1), inorganic silicon source is ethyl orthosilicate or methyl orthosilicate.
In above-mentioned steps (1), alkylol is the one or more in ethylene glycol, propylene glycol or glycerine.
In above-mentioned steps (1), alkali is ammonium hydroxide, the one or more of sodium hydroxide potassium hydroxide aqueous solution.
In above-mentioned steps (2), the template is any one in nonionic surfactant or cationic surfactant
Kind.Preferably, template is P123 or CnTAB, n=12-18.
The present invention, by one kettle way, fluorogen is introduced using the mode of copolycondensation using different compact nanometer particles as core
It is glimmering so as to be prepared for the modified nucleocapsid of shell skeleton organic fluorescence group into the shell inorganic skeleton of nucleocapsid silicon oxide nanoparticle
Light mesoporous silicon dioxide nano particle.
The beneficial effects of the present invention are：
(1) nucleocapsid fluorescence mesoporous inorganic oxide nano-particle of the present invention has big specific surface area and unimpeded duct system
System；
(2) there is regular pattern and good monodispersity；
(3) skeleton organic fluorescence group is modified, and fluorescence property is controllable；
(4) reaction condition is mild, prepares simple, easily repetition.
Description of the drawings
Fig. 1 is the core of embodiment 2 and the images of transmissive electron microscope (TEM) of core-shell particles that the present invention reports.
Fig. 2 is the small angle XRD (a) for the embodiment 2 that the present invention reports and nitrogen adsorption desorption curve (b).
Fig. 3 is the solid silicon evil spirit angle nuclear-magnetism (a) and fluorescence spectrum (b) of present invention report embodiment 2.
Specific embodiment
Below by embodiment, the present invention is further illustrated, and purpose, which is only that, is best understood from present disclosure
The protection domain being not intended to limit the present invention：
Examples 1 to 4
Core is changed for the preparation of the nucleocapsid fluorescence mesoporous monox nanometer particle of dense oxide silicon nano using mild
Into stober methods, by taking fluorogen is the sample of biphenyl as an example, specific preparation process is as follows：
1) preparation of dense oxide silicon core nano-particle：Ammonium hydroxide (2.56mL) and ethyl orthosilicate (TEOS, 1.42mL) one
It rises and is added in absolute ethyl alcohol (33mL), when reaction 24 is small.By reaction solution centrifuge washing, respectively washed with absolute ethyl alcohol and secondary water
For several times, product cake is collected, and is dried in vacuo at room temperature, obtains target nano-particle；
2) preparation of core-shell structure copolymer silicon oxide nanoparticle：Above-mentioned silicon oxide nanoparticle core (200mg) is suspended in absolute ethyl alcohol
In the mixed solution of (18mL) and secondary water (41mL), ultrasonic disperse adds in ammonium hydroxide (0.7mL) after twenty minutes, then adds pre-
What is first prepared contains cetyl ammonium bromide (CTAB, 0.24g, 0.66mmol), absolute ethyl alcohol (2mL) and secondary water (4mL)
Mixed liquor continue stirring 30 minutes, then to reaction solution add in TEOS (0.44mL) and biphenyl double end silicon source (100mg) continue instead
Answer 16 it is small when.Then by reacting liquid filtering, upper strata core-shell particles ethyl alcohol and secondary water centrifuge washing are multiple, then by particle room
The lower vacuum drying of temperature, vacuum preserves after grinding.
3) removal of shell mesopore orbit template：The core-shell structure copolymer nano-particle (50mg) of above-mentioned preparation is suspended in ethyl alcohol
(5mL) then adds in ammonium acetate (50mg, 0.64mmol), this mixed solution is heated to flowing back.After one hour, reaction solution is cold
But to room temperature, secondary water and the multiple filtering and washing of absolute ethyl alcohol, the drying of particle room temperature in vacuo.
It is made above to obtain being fluorescence mesoporous monox nanometer particle that fluorogen is biphenyl, organic double end silicon source with
The molar ratio of inorganic silicon source is 1:20 silicon oxide nanoparticle is denoted as embodiment 1.Embodiment 2-4 experimental procedures and embodiment 1
Identical, the organic double end silicon source weighed is different from the molar ratio of inorganic silicon source, and grain size is specific as follows all in 200nm or so：
| Embodiment | Double end silicon source:TEOS |
| Embodiment 1 | 1:20 |
| Embodiment 2 | 1:10 |
| Embodiment 3 | 1:5 |
| Embodiment 4 | 1:1 |
Embodiment 5-7
Core is equally changed for the preparation of the nucleocapsid fluorescence mesoporous monox nanometer particle of ferric oxide nano particles using mild
Into stober methods, by taking fluorogen is the sample of biphenyl as an example, specific preparation process is as follows：
1) preparation of dense oxide Fe nanometer particles：FeCl3.6H2O (0.85g), citric acid (0.48g), sodium acetate
(1.75g) is added in ethylene glycol (30mL), is transferred to water heating kettle after stirring a few hours, when 200 degree of reactions 10 are small, is cooled to room
Temperature after obtained black nano particle is washed for several times with absolute ethyl alcohol and deionized water, is scattered in ethyl alcohol.
2) preparation of core-shell structure copolymer inorganic nano-particle：Ferriferrous oxide nano-particle solution obtained above, takes 10mL to add in
Into the deionized water of 30mL, CTAB (40mg) is added, then adds in ammonium hydroxide (0.2mL), TEOS (100 μ L) and double end connection
Benzene silicon source (10 μ L) react at room temperature 10 it is small when, obtain core-shell particles ethyl alcohol and deionized water washing several times, vacuum protect
It deposits；
3) removal of shell mesopore orbit template：The core-shell structure copolymer nano-particle (50mg) of above-mentioned preparation is suspended in ethyl alcohol
(5mL) then adds in ammonium acetate (50mg, 0.64mmol), this mixed solution is heated to flowing back.After one hour, reaction solution is cold
But to room temperature, secondary water and the multiple filtering and washing of absolute ethyl alcohol, the drying of particle room temperature in vacuo.
The nucleocapsid fluorescence mesoporous silica nano particle that iron oxide is core is prepared according to above-described embodiment, is denoted as embodiment
5, embodiment 6-7 experimental procedures are same as Example 5, and the organic double end silicon source weighed is different from the molar ratio of inorganic silicon source, lead to
The molar ratio for crossing organic silicon source and inorganic silicon source regulates and controls, and the fluorescence property of fluorescent nano particles can be regulated and controled.
| Embodiment | Double end silicon source:TEOS |
| Embodiment 5 | 1:20 |
| Embodiment 6 | 1:10 |
| Embodiment 7 | 1:5 |
In the present invention, Fig. 1 is the core of the nano-particle of embodiment 2 and the scanning electron microscope (SEM) of core-shell particles and transmission electricity
Mirror image (TEM).Fig. 1 illustrates that the core of 2 nano-particle of embodiment and core-shell particles have good monodispersity and pattern, duct
Regular, nano particle diameter is about in 200nm or so.Fig. 2 is the small angle XRD (a) for 2 nano-particle of embodiment that the present invention reports
With nitrogen adsorption desorption curve (b).Fig. 2 illustrates that the nucleocapsid fluorescence silicon oxide nanoparticle prepared has the regular mesoporous knot of height
Structure, and even aperture distribution.Fig. 3 is the solid silicon evil spirit angle nuclear-magnetism (a) and fluorescence light of present invention report 2 nano-particle of embodiment
It composes (b).Fig. 3 illustrates the new nucleocapsid fluorescence silicon oxide nanoparticle prepared, is strictly introduced into organic fluorescence group (biphenyl)
In inorganic skeleton, and fluorescence property also keeps good.
The above is only the basic explanation under present inventive concept, and that technical solution according to the invention is done is any etc.
Effect conversion, is within the scope of protection of the invention.
Claims (5)
1. the preparation method of the fluorescence mesoporous inorganic oxide nano-particle of a kind of nucleocapsid, which is characterized in that fluorescence is mesoporous
The core of inorganic oxide nanoparticles is fine and close solid bead, in silica, iron oxide or manganese oxide inorganic nano-particle
Any one, shell is the group modified meso-hole structure of organic fluorescence；Specific preparation process is as follows：
(1) preparation of inorganic oxide nanoparticles
The inorganic oxide nano-particle is arbitrary in dense oxide silicon, compact iron oxide or dense oxide manganese inorganic nano-particle
It is a kind of；
(2) preparation of core-shell structure copolymer oxide nano-particles
The inorganic oxide nanoparticles of step (1) are suspended in absolute ethyl alcohol and the mixed solution of secondary water first, ultrasound
Adjusting PH with base is added in after scattered, the mixed liquor for being subsequently added into the template prepared in advance, absolute ethyl alcohol and secondary water continues to stir,
Inorganic silicon source and the compound reaction containing organic fluorescent chromophore are added in into reaction solution again；Finally by reacting liquid filtering, upper strata
Core-shell particles washing is dried in vacuo at room temperature, is ground；Wherein：The compound containing organic fluorescent chromophore is organic fluorescence
Double end silicon source structure, representation are (R ' O)3Si-R-Si(R’O)3, wherein R ' is C1-C4Alkyl, R are fluorescent chromophore；
(3) removal of shell mesopore orbit template
The core-shell structure copolymer oxide nano-particles that step (2) obtains are suspended in ethyl alcohol, then add in ammonium acetate, this mixing is molten
Liquid is heated to flowing back, when 1-2 is small after, reaction solution is cooled to room temperature, and is filtered, is washed, particle room temperature in vacuo drying, obtain nucleocapsid knot
The fluorescence mesoporous inorganic oxide nano-particle of structure；Wherein：The rate of charge of nano-particle and ethyl alcohol is (50~10000):(5~
5000)mg/mL。
2. preparation method according to claim 1, which is characterized in that in step (1), inorganic oxide nanoparticles are to cause
During close silicon oxide nanoparticle, it is prepared via a method which to obtain：
Alkali is added to together with inorganic silicon source in alkylol, when reaction 10~24 is small, by reaction solution centrifuge washing, uses absolute ethyl alcohol
It is respectively washed with secondary water for several times, collects product cake, and be dried in vacuo at room temperature, obtain target nano-particle；Alkali, inorganic silicon source
And the volume ratio that feeds intake (2.56~100) of alkylol:(1.42~200):(33~3000)；
When the inorganic oxide nanoparticles are dense oxide Fe nanometer particles, it is prepared via a method which to obtain：
By FeCl3, citric acid, sodium acetate, be added in alkylol, be transferred to water heating kettle after stirring, 200~300 DEG C of reactions 10~
24 it is small when, be cooled to room temperature, after obtained black nano particle is washed for several times with absolute ethyl alcohol and deionized water, be scattered in ethyl alcohol
In；Wherein：FeCl3, citric acid and sodium acetate mass ratio be (85~2000):(48~3000):(1.75~500)；FeCl3
Mass volume ratio with alkylol is (85~2000)：(300~40000) mg/mL.
3. preparation method according to claim 2, which is characterized in that inorganic silicon source is ethyl orthosilicate or positive silicic acid first
Ester；Alkali is ammonium hydroxide, the one or more of sodium hydroxide potassium hydroxide aqueous solution；The alkylol is ethylene glycol, propylene glycol
Or the one or more in glycerine.
4. preparation method according to claim 1, which is characterized in that in step (2), the template is non-ionic surface
Any one in activating agent or cationic surfactant.
5. preparation method according to claim 1, which is characterized in that in step (2), the template for P123 or
CnTAB, n=12-18.
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