CN105315990B - A kind of preparation method of organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial - Google Patents
A kind of preparation method of organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial, the method includes：, as carrier, pre-processed from double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size；Dual model mesoporous silicon oxide nanomaterial after treatment is mixed with the dichloromethane solution containing organic fluorescence molecule, condensing reflux 8~12 hours；After the completion of reaction, through centrifugation, washing, dry, obtain organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial.A kind of preparation method of organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial disclosed by the invention, preparation process is simple, low cost is easy to operate；The organic inorganic hybridization fluorescent mesoporous silicon oxide nanomaterial for preparing has preferably dispersed, more uniform nano-scale and adjustable aperture, and fluorescence intensity is high, good stability.
Description
Technical field
Received the present invention relates to fluorescent nano material field, more particularly to a kind of hybrid inorganic-organic fluorescence mesopore silicon oxide
The preparation method of rice material.
Background technology
Mesoporous material is a kind of novel nano porous material for growing up at the beginning of the nineties in last century, with surfactant point
Sub- aggregation is template, and the regular nothing of the pore passage structure for generating is assembled by the interface interaction between organic matter and inorganic matter
Machine porous material.Due to containing a large amount of hydroxyls with larger specific surface area and pore volume, morphology controllable, regular pore structure and surface
The features such as base (- OH) and easily functionalization, synthesis and the application of mesoporous material have become one of study hotspot of people.With glimmering
The mesoporous material of optical property, has wide at aspects such as medicament slow release, medical diagnosis on disease, analysis detection, cell marking and genophores
Wealthy application prospect.
Bipyridyl and its derivative are the important organic heterocyclic molecules of a class, not only with good bioactivity, point
Electronics and energy transmission property etc. in sub, also with special magnetic, optical physics and electrochemical properties, therefore in organic optoelectronic and
Bio-sensing aspect has good potential application, but it has the disadvantage that photo and thermal stability is poor as fluorescence organic molecule,
Easily reunite and cause fluorescent quenching.With the development of nanometer technology, it has been found that be carried in inorganic carrier duct, mesoporous hole
Road characteristic in itself can avoid organic fluorescence molecule from reuniting, and reach high degree of dispersion state, and using the hydroxyl on silica-base material surface
Base is acted on, and can improve fluorescence intensity and photostability.(J.Phys.Chem., 1992,96 such as Dutta:9410-9416) pass through
Ion exchange will contain ruthenium species and be introduced into Y type molecular sieve, then the ruthenium material and 2 under 200 DEG C of vacuum conditions, 2 '-bipyridyl hair
Raw solid phase reaction, removes reaction raw materials, and then obtain Ru (bpy) by way of liquid-solid extraction3 2+The molecular sieve of filling, but
Easily there is the phenomenon such as fluorescent quenching and lifetime of excited state reduction in the material.(Southeast China University's journal, 2005,21 such as Ge Shuxun
(2):211-214) assembled in Mesoporous silica MCM 41 under bipyridyl europium, but MCM-41 meso-hole structure orders using infusion process
Drop is obvious.Patent CN101864291A comes with tris (bipyridine) ruthenium as kernel in the silica of its surface covering network structure
To Ru (bpy)3/SiO2Fluorescent nano particles；With patent CN1621486A is formed from bipyridyl and its derivative and metal Ru
Thing is compounded to form luminescent material with inorganic mesoporous molecular sieve (MCM-41, MCM-48).Above fluorescent material is all by forming gold
Metal complex distich pyridine and its derivatives are loaded, and slaine is relatively costly in complex operation and preparation process.
The content of the invention
Weak point present in regarding to the issue above, the present invention provides a kind of mesoporous oxidation of hybrid inorganic-organic fluorescence
The preparation method of silicon nano material.
The invention discloses a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial, the method
Including：
Step one, from double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size as load
Body, is pre-processed；
Step 2, by the dual model mesoporous silicon oxide nanomaterial after treatment and the dichloromethane containing organic fluorescence molecule
Solution mixes, condensing reflux 8~12 hours；
After the completion of step 3, reaction, through centrifugation, washing, dry, obtain hybrid inorganic-organic fluorescence mesopore silicon oxide and receive
Rice material.
As a further improvement on the present invention, the dual model mesoporous silicon oxide nanomaterial have 2~4nm mesoporous and
The spheric granules of 10~30nm piles up hole.
As a further improvement on the present invention, the double-pore structure and controllable dual model of pore size is mesoporous in the step one
Aoxidize silicon nano material preparation method be：
By quaternary surfactant CnH2n+1(CH3)3NBr (n=12,14,16,18) is with distilled water according to 1:800 rub
You mix ratio, stirring to dissolving；
To tetraethyl orthosilicate is pipetted in solution, tetraethyl orthosilicate is 1 with the molar ratio of quaternary surfactant：(0.1
~0.3)；
Ammoniacal liquor is added to adjust the pH to 8~11 of solution, stirring to generation white chunks gel；
Filtering, washing, dry, the white powder of gained is calcined at 550 DEG C of temperature, obtain dual model mesopore silicon oxide
Nano material.
As a further improvement on the present invention, the method for pretreatment is in the step one：Dual model mesopore silicon oxide is received
Rice material is activated 3 hours for 120 DEG C in vacuum.
As a further improvement on the present invention, the organic fluorescence molecule is the one kind in dipyridyl derivatives class, joins pyrrole
The molecular structure of piperidine derivatives is：
Wherein R represents H, L-PROLINE, N- benzyloxycarbonyl groups-prolineamide, 3-CH3C6H4CO, (CH3)3CO or CH3CO。
As a further improvement on the present invention, the matter of the organic fluorescence molecule and dual model mesoporous silicon oxide nanomaterial
Amount is than being (0.1-30)：100.
As a further improvement on the present invention, in the step 2 dual model mesoporous silicon oxide nanomaterial with containing organic
The temperature of the dichloromethane solution reaction of fluorescence molecule is 40~45 DEG C.
Compared with prior art, beneficial effects of the present invention are：
A kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed by the invention, prepares work
Skill is simple, and low cost is easy to operate；The hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial for preparing has preferable
Dispersed, more uniform nano-scale and adjustable aperture, fluorescence intensity is high, good stability.
Brief description of the drawings
Fig. 1 is the preparation of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed in an embodiment of the present invention
The flow chart of method；
Fig. 2 is the ESEM of fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-15 " sample of preparation in embodiment 1
Photo；
Fig. 3 is the fluorescence spectra of the fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-30 " of preparation in embodiment 6；
Fig. 4 is that the nitrogen adsorption desorption of the fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-30 " of preparation in embodiment 6 is bent
Line and pore-size distribution schematic diagram.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill people
The every other embodiment that member is obtained on the premise of creative work is not made, belongs to the scope of protection of the invention.
As shown in figure 1, the invention discloses a kind of preparation side of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial
Method, the method includes：
S101, from double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size as load
Body, is pre-processed；
S102, dual model mesoporous silicon oxide nanomaterial is mixed with the dichloromethane solution containing organic fluorescence molecule,
Dichloromethane is as the solvent for dissolving organic fluorescence molecule, it is ensured that dispersion of the organic fluorescence molecule in dichloromethane solution
Property, condensing reflux 8~12 hours；
After the completion of S103, reaction, through centrifugation, washing, dry, obtain hybrid inorganic-organic fluorescence mesoporous monox nanometer
Material.
Further, dual model mesoporous silicon oxide nanomaterial has mesoporous and 10~30nm the spheric granules heap of 2~4nm
Product hole.
Further, in S101 double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size preparation side
Method is：
By quaternary surfactant CnH2n+1(CH3)3NBr (n=12,14,16,18) is with distilled water according to 1:800 rub
You mix ratio, stirring to dissolving；
To tetraethyl orthosilicate is pipetted in solution, tetraethyl orthosilicate is 1 with the molar ratio of quaternary surfactant：(0.1
~0.3)；
Ammoniacal liquor is added to adjust the pH to 8~11 of solution, stirring to generation white chunks gel；
Filtering, washing, dry, the white powder of gained is calcined at 550 DEG C of temperature, obtain dual model mesopore silicon oxide
Nano material.
Further, the method for pretreatment is in S101：Dual model mesoporous silicon oxide nanomaterial is in 120 DEG C of activation 3 of vacuum
Hour.
Further, organic fluorescence molecule is the one kind in dipyridyl derivatives class, and the molecular structure of dipyridyl derivatives is：
Wherein R represents H, L-PROLINE, N- benzyloxycarbonyl groups-prolineamide, 3-CH3C6H4CO, (CH3)3CO, or CH3CO；Have
Machine fluorescence molecule is H, L-PROLINE, N- benzyloxycarbonyl groups-prolineamide, 3-CH from R3C6H4CO、(CH3)3CO or CH3CO's
One kind in dipyridyl derivatives class.
Further, organic fluorescence molecule and the mass ratio of dual model mesoporous silicon oxide nanomaterial are (0.1-30)：100.
Further, dual model mesoporous silicon oxide nanomaterial and the dichloromethane solution containing organic fluorescence molecule in S102
The temperature of reaction is 40~45 DEG C.
The present invention is described in further detail below in conjunction with the accompanying drawings：
Embodiment 1：
2.61g cetyl trimethylammonium bromides are dissolved in 104g distilled water, stirring to dissolving, to pipetting 8mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.4mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains the dual model mesoporous molecular that the mesoporous and 16nm spheric granules with 3nm piles up hole
Sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
The dichloromethane solution of 0.045g organic fluorescence molecules Z1 (R group is L-PROLINE), dichloromethane is organic glimmering as dissolving
The solvent of optical molecule, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches 41 DEG C, it is ensured that two
Chloromethanes solution is seethed with excitement, and after condensing reflux 12h, centrifugation, washing is dried, and gained solid powder is fluorescence mesopore silicon oxide and receives
Rice material Z1-BMMs-15, its Fluorescent peal is at 499nm；Its scanning electron microscope (SEM) photograph is as shown in Figure 2.
Embodiment 2：
Using the experimentation of embodiment 1, it is to add 3mL to contain 0.0003g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-0.1, its Fluorescent peal in
At 491nm.
Embodiment 3：
Using the experimentation of embodiment 1, it is to add 3mL to contain 0.003g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-1, its Fluorescent peal in
At 493nm.
Embodiment 4：
Using the experimentation of embodiment 1, it is to add 3mL to contain 0.009g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-3, its Fluorescent peal in
At 496nm.
Embodiment 5：
Using the experimentation of embodiment 1, it is to add 3mL to contain 0.03g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-10, its Fluorescent peal in
At 498nm.
Embodiment 6：
Using the experimentation of embodiment 1, it is to add 3mL to contain 0.09g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-30, as shown in figure 3, its is glimmering
Photopeak is at 500nm.
As can be seen that the nitrogen adsorption desorption curve of sample Z1-BMMs-30 is IV type thermoisopleths from accompanying drawing 4, i.e., with allusion quotation
The meso-hole structure of type.Adsorption desorption curve shows two hysteresis loops, and first occurs in low-pressure area, first through nitrogen individual layer and multilayer
Absorption, adsorption curve slowly rises；In relative pressure P/P0Between 0.30~0.40, nitrogen adsorption curve suddenly rises, hair
Raw capillary condensation, corresponding to one-level hole adsorption desorption, second steeper hysteresis loop occurs in higher-pressure region relative pressure P/P0
Between 0.80~0.98, corresponding to capillary condensation of the generation in particle packing hole.With reference to pore distribution curve, it can be seen that
Z1-BMMs-30 has double-pore structure, and one-level hole most probable pore size (mesoporous pore size) is 2.7nm, particle packing most probable pore size
(particle packing hole aperture) is 15.8nm.
Embodiment 7：
2.81g Cetyltrimethylammonium bromides are dissolved in 104g distilled water, stirring to dissolving, to pipetting 8mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.4mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains mesoporous point of the dual model that the mesoporous and 18nm spheric granules with 3.2nm piles up hole
Son sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
The dichloromethane solution of 0.045g organic fluorescence molecules Z2 (R group is H), dichloromethane is as the organic fluorescence molecule of dissolving
Solvent, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches 41 DEG C, it is ensured that dichloromethane is molten
Liquid is seethed with excitement, and after condensing reflux 12h, centrifugation, washing is dried, and gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z2-
BMMs-15, its Fluorescent peal is at 499nm.
Embodiment 8：
Using the experimentation of embodiment 7, it is to add 3mL to contain 0.003g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z2-BMMs-1, its Fluorescent peal in
At 493nm.
Embodiment 9：
Using the experimentation of embodiment 7, it is to add 3mL to contain 0.09g organic fluorescence molecules to be different from part
Dichloromethane solution, gained solid powder is fluorescent mesoporous silicon oxide nanomaterial Z2-BMMs-30, its Fluorescent peal in
At 500nm.
Embodiment 10：
2.21g DTABs are dissolved in 104g distilled water, stirring to dissolving, to pipetting 10mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.5mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains the dual model mesoporous molecular that the mesoporous and 18nm spheric granules with 3nm piles up hole
Sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
The dichloromethane solution of 0.045g organic fluorescence molecules Z3 (R group is N- benzyloxycarbonyl groups-prolineamide), dichloromethane is in conduct
Dissolve the solvent of organic fluorescence molecule, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches
42 DEG C, it is ensured that dichloromethane solution seethes with excitement, after condensing reflux 10h, centrifugation, washing is dried, and gained solid powder is fluorescence Jie
Hole aoxidizes silicon nano material Z3-BMMs-15, and its Fluorescent peal is at 498nm.
Embodiment 11：
2.41g TTABs are dissolved in 104g distilled water, stirring to dissolving, to pipetting 10mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.5mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains mesoporous point of the dual model that the mesoporous and 16nm spheric granules with 2.5nm piles up hole
Son sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
(R group is 3-CH to 0.045g organic fluorescence molecules Z43C6H4CO dichloromethane solution), dichloromethane is organic as dissolving
The solvent of fluorescence molecule, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches 41 DEG C, it is ensured that
Dichloromethane solution is seethed with excitement, and after condensing reflux 8h, centrifugation, washing is dried, and gained solid powder is fluorescence mesopore silicon oxide and receives
Rice material Z4-BMMs-15, its Fluorescent peal is at 495nm.
Embodiment 12：
2.41g TTABs are dissolved in 104g distilled water, stirring to dissolving, to pipetting 12mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.8mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains mesoporous point of the dual model that the mesoporous and 16nm spheric granules with 2.6nm piles up hole
Son sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
(R group is (CH to 0.045g organic fluorescence molecules Z53)3CO dichloromethane solution), dichloromethane is as dissolving organic fluorescence
The solvent of molecule, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches 42 DEG C, it is ensured that dichloro
Dichloromethane is seethed with excitement, and after condensing reflux 10h, centrifugation, washing is dried, and gained solid powder is fluorescence mesoporous monox nanometer
Material Z5-BMMs-15, its Fluorescent peal is at 496nm.
Embodiment 13：
2.41g TTABs are dissolved in 104g distilled water, stirring to dissolving, to pipetting 10mL in solution
Tetraethyl orthosilicate, adds brand-new ammoniacal liquor 2.4mL, and to white chunks gel is produced, filtering, washing is dried for stirring, gained white powder
End is warming up to 550 DEG C and calcines 5 hours, obtains mesoporous point of the dual model that the mesoporous and 16nm spheric granules with 2.5nm piles up hole
Son sieve.
0.3g dual models mesopore molecular sieve is taken in 25mL round-bottomed flasks, 120 DEG C of activation 3h of vacuum add 3mL to contain
(R group is CH to 0.045g organic fluorescence molecules Z63CO dichloromethane solution), dichloromethane is as dissolving organic fluorescence point
The solvent of son, it is ensured that dispersiveness of the organic fluorescence molecule in dichloromethane solution；Heating-up temperature reaches 41 DEG C, it is ensured that dichloromethane
Alkane solution is seethed with excitement, and after condensing reflux 10h, centrifugation, washing is dried, and gained solid powder is fluorescence mesoporous monox nanometer material
Material Z6-BMMs-15, its Fluorescent peal is at 495nm.
A kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed by the invention, prepares work
Skill is simple, and low cost is easy to operate；The hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial for preparing has preferable
Dispersed, more uniform nano-scale and adjustable aperture, mesoporous pore size adjustable extent is ensured by the setting of preparation parameter
It is 2~4nm, accumulation hole aperture adjustable extent is 10~30nm, fluorescence intensity is high, good stability.
The preferred embodiments of the present invention are these are only, is not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial, it is characterised in that the method bag
Include：
Step one, from double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size as carrier,
Pre-processed；The method of pretreatment is：Dual model mesoporous silicon oxide nanomaterial is activated 3 hours for 120 DEG C in vacuum；
Step 2, by the dual model mesoporous silicon oxide nanomaterial after treatment and the dichloromethane solution containing dipyridyl derivatives
Mixing, condensing reflux 8~12 hours；
After the completion of step 3, reaction, through centrifugation, washing, dry, obtain hybrid inorganic-organic fluorescence mesoporous monox nanometer material
Material.
2. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, its feature exists
In mesoporous and 10~30nm the spheric granules that the dual model mesoporous silicon oxide nanomaterial has 2~4nm piles up hole.
3. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, its feature exists
In the preparation method of double-pore structure and the controllable dual model mesoporous silicon oxide nanomaterial of pore size is in the step one：
By quaternary surfactant CnH2n+1(CH3)3NBr, n=12,14,16,18, with distilled water according to 1:800 mol ratio
Example mixing, stirring to dissolving；
To tetraethyl orthosilicate is pipetted in solution, tetraethyl orthosilicate is 1 with the molar ratio of quaternary surfactant：(0.1~
0.3)；
Ammoniacal liquor is added to adjust the pH to 8~11 of solution, stirring to generation white chunks gel；
Filtering, washing, dry, the white powder of gained is calcined at 550 DEG C of temperature, obtain dual model mesoporous monox nanometer
Material.
4. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, its feature exists
In the molecular structure of the dipyridyl derivatives is：
Wherein R represents H, L-PROLINE, N- benzyloxycarbonyl groups-prolineamide, 3-CH3C6H4CO, (CH3)3CO or CH3CO。
5. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, its feature exists
In the dipyridyl derivatives are (0.1-30) with the mass ratio of dual model mesoporous silicon oxide nanomaterial：100.
6. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, its feature exists
In dual model mesoporous silicon oxide nanomaterial and the dichloromethane solution reaction containing dipyridyl derivatives in the step 2
Temperature is 40~45 DEG C.
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