CN105315990A - Method for preparing organic-inorganic hybrid fluorescent mesoporous silica nanometer material - Google Patents
Method for preparing organic-inorganic hybrid fluorescent mesoporous silica nanometer material Download PDFInfo
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Abstract
The invention discloses a method for preparing an organic-inorganic hybrid fluorescent mesoporous silica nanometer material. The method comprises the following steps: selecting a dual model mesoporous silica nanometer material with a dual pore structure and a controllable pore size as a carrier, and performing pretreatment; mixing the treated dual model mesoporous silica nanometer material and a dichloromethane solution containing organic fluorescence molecules, and performing reflux condensation for 8-12 hours; and centrifuging, washing and drying after the reaction is finished, thereby obtaining the organic-inorganic hybrid fluorescent mesoporous silica nanometer material. According to the method for preparing the organic-inorganic hybrid fluorescent mesoporous silica nanometer material, disclosed by the invention, the preparation process is simple, the cost is low, and the operation is simple and convenient. Moreover, the prepared organic-inorganic hybrid fluorescent mesoporous silica nanometer material has the advantages of high dispersity, uniform nanometer size, adjustable pore diameter, high fluorescence intensity and high stability.
Description
Technical field
The present invention relates to fluorescent nano material field, particularly relate to a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial.
Background technology
Mesoporous material is a kind of novel nano porous material grown up the beginning of the nineties in last century, with surfactant molecules aggregate body for template, and the inorganic porous material that the pore passage structure generated by the interface interaction assembling between organism and inorganics is regular.Owing to having larger specific surface area and pore volume, morphology controllable, regular pore structure and surface containing great amount of hydroxy group (-OH) and the easily feature such as functionalized, Synthesis and application one of study hotspot becoming people of mesoporous material.There is the mesoporous material of fluorescence property, have broad application prospects in medicament slow release, medical diagnosis on disease, analyzing and testing, cell marking and genophore etc.
Dipyridyl and derivative thereof are the important organic heterocyclic molecules of a class, not only there is electronics and transmission ofenergy character etc. in good biological activity, molecule, also there is special magnetic, optical physics and electrochemical properties, therefore there is good potential application in organic optoelectronic and bio-sensing, but be that photo and thermal stability is poor as its shortcoming of fluorescence organic molecule, easily reuniting causes quenching of fluorescence.Along with the development of nanotechnology, it is found that and be carried in inorganic carrier duct, the characteristic of mesopore orbit itself can avoid organic fluorescence molecule to reunite, and reaches high dispersing state, and utilize the hydroxyl effect on silica-base material surface, fluorescence intensity and light stability can be improved.(the J.Phys.Chem. such as Dutta, 1992,96:9410-9416) will introduce in Y zeolite containing ruthenium species by ion-exchange, then ruthenium material and 2 under 200 DEG C of vacuum conditions, 2 '-dipyridyl generation solid state reaction, remove reaction raw materials by the mode of liquid-solid extraction, and then obtain Ru (bpy)
3 2+the molecular sieve of filling, but easily there is the phenomenon such as fluorescent quenching and lifetime of excited state reduction in this material.Ge Shuxun etc. (Southeast China University's journal, 2005,21 (2): 211-214) adopt pickling process in Mesoporous silica MCM 41, assemble dipyridyl europium, but MCM-41 meso-hole structure order declines obviously.Patent CN101864291A take tris (bipyridine) ruthenium as kernel, obtains Ru (bpy) at the cancellated silicon-dioxide of its surface coverage
3/ SiO
2fluorescent nano particles; The title complex that patent CN1621486A is formed by dipyridyl and derivative thereof and metal Ru is compounded to form luminescent material with inorganic mesoporous molecular sieve (MCM-41, MCM-48).Above fluorescent material is all carry out load by forming metal complexes distich pyridine and its derivatives, complicated operation and in preparation process metal-salt cost higher.
Summary of the invention
For the weak point existed in the problems referred to above, the invention provides a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial.
The invention discloses a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial, the method comprises:
Step one, select there is double-pore structure and the controlled dual model mesoporous silicon oxide nanomaterial of pore size as carrier, carry out pre-treatment;
Step 2, by process after dual model mesoporous silicon oxide nanomaterial mix with the dichloromethane solution containing organic fluorescence molecule, condensing reflux 8 ~ 12 hours;
Step 3, reacted after, through centrifugal, washing, dry, obtain hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial.
As a further improvement on the present invention, described dual model mesoporous silicon oxide nanomaterial has the spheroidal particle accumulation hole of the mesoporous of 2 ~ 4nm and 10 ~ 30nm.
As a further improvement on the present invention, in described step one, double-pore structure and the preparation method of the controlled dual model mesoporous silicon oxide nanomaterial of pore size are:
By quaternary surfactant C
nh
2n+1(CH
3)
3nBr (n=12,14,16,18) mixes with the molar ratio of distilled water according to 1:800, is stirred to dissolving;
In solution, pipette tetraethoxy, the molar ratio of tetraethoxy and quaternary surfactant is 1:(0.1 ~ 0.3);
Add pH to 8 ~ 11 of ammoniacal liquor regulator solution, be stirred to and produce white chunks gel;
Filtration, washing, drying, calcine the white powder of gained, obtain dual model mesoporous silicon oxide nanomaterial at temperature 550 DEG C.
As a further improvement on the present invention, in described step one, pretreated method is: dual model mesoporous silicon oxide nanomaterial was 120 DEG C, vacuum activation 3 hours.
As a further improvement on the present invention, described organic fluorescence molecule is the one in dipyridyl derivatives class, and the molecular structure of dipyridyl derivatives is:
Wherein R represents H, L-PROLINE, N-carbobenzoxy-(Cbz)-prolineamide, 3-CH
3c
6h
4cO, (CH
3)
3cO or CH
3cO.
As a further improvement on the present invention, the mass ratio of described organic fluorescence molecule and dual model mesoporous silicon oxide nanomaterial is (0.1-30): 100.
As a further improvement on the present invention, the temperature that in described step 2, dual model mesoporous silicon oxide nanomaterial and the dichloromethane solution containing organic fluorescence molecule react is 40 ~ 45 DEG C.
Compared with prior art, beneficial effect of the present invention is:
The preparation method of a kind of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed by the invention, preparation technology is simple, and cost is low, easy and simple to handle; The hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial prepared has good dispersiveness, more homogeneous nano-scale and adjustable aperture, and fluorescence intensity is high, good stability.
Accompanying drawing explanation
The schema of Fig. 1 preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed in an embodiment of the present invention;
Fig. 2 is the stereoscan photograph of fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-15 " sample of preparation in embodiment 1;
Fig. 3 is the fluorescence spectrum figure of the fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-30 " of preparation in embodiment 6;
Fig. 4 is nitrogen adsorption desorption curve and the pore size distribution schematic diagram of the fluorescent mesoporous silicon oxide nanomaterial " Z1-BMMs-30 " of preparation in embodiment 6.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
As shown in Figure 1, the invention discloses a kind of preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial, the method comprises:
S101, select there is double-pore structure and the controlled dual model mesoporous silicon oxide nanomaterial of pore size as carrier, carry out pre-treatment;
S102, dual model mesoporous silicon oxide nanomaterial to be mixed with the dichloromethane solution containing organic fluorescence molecule, methylene dichloride is at the solvent as the organic fluorescence molecule of dissolving, ensure the dispersiveness of organic fluorescence molecule in dichloromethane solution, condensing reflux 8 ~ 12 hours;
S103, reacted after, through centrifugal, washing, dry, obtain hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial.
Further, dual model mesoporous silicon oxide nanomaterial has the spheroidal particle accumulation hole of the mesoporous of 2 ~ 4nm and 10 ~ 30nm.
Further, in S101, double-pore structure and the preparation method of the controlled dual model mesoporous silicon oxide nanomaterial of pore size are:
By quaternary surfactant C
nh
2n+1(CH
3)
3nBr (n=12,14,16,18) mixes with the molar ratio of distilled water according to 1:800, is stirred to dissolving;
In solution, pipette tetraethoxy, the molar ratio of tetraethoxy and quaternary surfactant is 1:(0.1 ~ 0.3);
Add pH to 8 ~ 11 of ammoniacal liquor regulator solution, be stirred to and produce white chunks gel;
Filtration, washing, drying, calcine the white powder of gained, obtain dual model mesoporous silicon oxide nanomaterial at temperature 550 DEG C.
Further, in S101, pretreated method is: dual model mesoporous silicon oxide nanomaterial was 120 DEG C, vacuum activation 3 hours.
Further, organic fluorescence molecule is the one in dipyridyl derivatives class, and the molecular structure of dipyridyl derivatives is:
Wherein R represents H, L-PROLINE, N-carbobenzoxy-(Cbz)-prolineamide, 3-CH
3c
6h
4cO, (CH
3)
3cO, or CH
3cO; Organic fluorescence molecule selects R to be H, L-PROLINE, N-carbobenzoxy-(Cbz)-prolineamide, 3-CH
3c
6h
4cO, (CH
3)
3cO or CH
3one in the dipyridyl derivatives class of CO.
Further, the mass ratio of organic fluorescence molecule and dual model mesoporous silicon oxide nanomaterial is (0.1-30): 100.
Further, the temperature that in S102, dual model mesoporous silicon oxide nanomaterial and the dichloromethane solution containing organic fluorescence molecule react is 40 ~ 45 DEG C.
Below in conjunction with accompanying drawing, the present invention is described in further detail:
Embodiment 1:
2.61g cetyl trimethylammonium bromide is dissolved in 104g distilled water, be stirred to dissolving, 8mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.4mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 3nm and 16nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, add the dichloromethane solution that 3mL contains 0.045g organic fluorescence molecule Z1 (R group is L-PROLINE), methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 41 DEG C, ensures dichloromethane solution boiling, after condensing reflux 12h, centrifugal, washing, and dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-15, and its Fluorescent peal is in 499nm place; Its scanning electron microscope (SEM) photograph as shown in Figure 2.
Embodiment 2:
Adopt the experimentation of embodiment 1, be with its difference, add the dichloromethane solution that 3mL contains 0.0003g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-0.1, and its Fluorescent peal is in 491nm place.
Embodiment 3:
Adopt the experimentation of embodiment 1, be with its difference, add the dichloromethane solution that 3mL contains 0.003g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-1, and its Fluorescent peal is in 493nm place.
Embodiment 4:
Adopt the experimentation of embodiment 1, be with its difference, add the dichloromethane solution that 3mL contains 0.009g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-3, and its Fluorescent peal is in 496nm place.
Embodiment 5:
Adopt the experimentation of embodiment 1, be with its difference, add the dichloromethane solution that 3mL contains 0.03g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-10, and its Fluorescent peal is in 498nm place.
Embodiment 6:
Adopt the experimentation of embodiment 1, be with its difference, add the dichloromethane solution that 3mL contains 0.09g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z1-BMMs-30, as shown in Figure 3, its Fluorescent peal is in 500nm place.
As can be seen from accompanying drawing 4, the nitrogen adsorption desorption curve of sample Z1-BMMs-30 is IV type thermoisopleth, namely has typical meso-hole structure.Adsorption desorption curve table reveals two hysteresis loops, and first occurs in low pressure area, and first through nitrogen individual layer and multilayer absorption, adsorption curve slowly rises; At relative pressure P/P
0between 0.30 ~ 0.40, nitrogen adsorption curve suddenly rises, and capillary condensation occurs, and corresponding to one-level hole adsorption desorption, second steeper hysteresis loop occurs in high pressure area relative pressure P/P
0between 0.80 ~ 0.98, corresponding to the capillary condensation occurred in particle packing hole.Combined hole distribution curve, can find out that Z1-BMMs-30 has double-pore structure, and one-level hole most probable pore size (mesoporous pore size) is 2.7nm, and particle packing most probable pore size (aperture, particle packing hole) is 15.8nm.
Embodiment 7:
2.81g Cetyltrimethylammonium bromide is dissolved in 104g distilled water, be stirred to dissolving, 8mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.4mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 3.2nm and 18nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, add the dichloromethane solution that 3mL contains 0.045g organic fluorescence molecule Z2 (R group is H), methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 41 DEG C, ensures dichloromethane solution boiling, after condensing reflux 12h, centrifugal, and washing, dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z2-BMMs-15, and its Fluorescent peal is in 499nm place.
Embodiment 8:
Adopt the experimentation of embodiment 7, be with its difference, add the dichloromethane solution that 3mL contains 0.003g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z2-BMMs-1, and its Fluorescent peal is in 493nm place.
Embodiment 9:
Adopt the experimentation of embodiment 7, be with its difference, add the dichloromethane solution that 3mL contains 0.09g organic fluorescence molecule, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z2-BMMs-30, and its Fluorescent peal is in 500nm place.
Embodiment 10:
2.21g Trimethyllaurylammonium bromide is dissolved in 104g distilled water, be stirred to dissolving, 10mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.5mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 3nm and 18nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, add the dichloromethane solution that 3mL contains 0.045g organic fluorescence molecule Z3 (R group is N-carbobenzoxy-(Cbz)-prolineamide), methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 42 DEG C, ensures dichloromethane solution boiling, after condensing reflux 10h, centrifugal, and washing, dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z3-BMMs-15, and its Fluorescent peal is in 498nm place.
Embodiment 11:
2.41g Tetradecyl Trimethyl Ammonium Bromide is dissolved in 104g distilled water, be stirred to dissolving, 10mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.5mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 2.5nm and 16nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, adds 3mL and contains 0.045g organic fluorescence molecule Z4 (R group is 3-CH
3c
6h
4cO) dichloromethane solution, methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 41 DEG C, ensures dichloromethane solution boiling, after condensing reflux 8h, centrifugal, and washing, dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z4-BMMs-15, and its Fluorescent peal is in 495nm place.
Embodiment 12:
2.41g Tetradecyl Trimethyl Ammonium Bromide is dissolved in 104g distilled water, be stirred to dissolving, 12mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.8mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 2.6nm and 16nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, add 3mL and contain 0.045g organic fluorescence molecule Z5 (R group is for (CH
3)
3cO) dichloromethane solution, methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 42 DEG C, ensures dichloromethane solution boiling, after condensing reflux 10h, centrifugal, and washing, dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z5-BMMs-15, and its Fluorescent peal is in 496nm place.
Embodiment 13:
2.41g Tetradecyl Trimethyl Ammonium Bromide is dissolved in 104g distilled water, be stirred to dissolving, 10mL tetraethoxy is pipetted in solution, add brand-new ammoniacal liquor 2.4mL, be stirred to and produce white chunks gel, filter, washing, drying, gained white powder is warming up to 550 DEG C of calcinings 5 hours, obtains the dual model mesopore molecular sieve with the mesoporous of 2.5nm and 16nm spheroidal particle accumulation hole.
Get 0.3g dual model mesopore molecular sieve in 25mL round-bottomed flask, 120 DEG C, vacuum activation 3h, adds 3mL and contains 0.045g organic fluorescence molecule Z6 (R group is CH
3cO) dichloromethane solution, methylene dichloride, as the solvent dissolving organic fluorescence molecule, ensures the dispersiveness of organic fluorescence molecule in dichloromethane solution; Heating temperature reaches 41 DEG C, ensures dichloromethane solution boiling, after condensing reflux 10h, centrifugal, and washing, dry, gained pressed powder is fluorescent mesoporous silicon oxide nanomaterial Z6-BMMs-15, and its Fluorescent peal is in 495nm place.
The preparation method of a kind of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial disclosed by the invention, preparation technology is simple, and cost is low, easy and simple to handle; The hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial prepared has good dispersiveness, more homogeneous nano-scale and adjustable aperture, ensure that mesoporous pore size variable range is 2 ~ 4nm by the setting of preparation parameter, piling up aperture, hole variable range is 10 ~ 30nm, fluorescence intensity is high, good stability.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a preparation method for hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial, is characterized in that, the method comprises:
Step one, select there is double-pore structure and the controlled dual model mesoporous silicon oxide nanomaterial of pore size as carrier, carry out pre-treatment;
Step 2, by process after dual model mesoporous silicon oxide nanomaterial mix with the dichloromethane solution containing organic fluorescence molecule, condensing reflux 8 ~ 12 hours;
Step 3, reacted after, through centrifugal, washing, dry, obtain hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial.
2. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, is characterized in that, the spheroidal particle that described dual model mesoporous silicon oxide nanomaterial has the mesoporous of 2 ~ 4nm and 10 ~ 30nm piles up hole.
3. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, is characterized in that, double-pore structure in described step one and the preparation method of the controlled dual model mesoporous silicon oxide nanomaterial of pore size are:
By quaternary surfactant C
nh
2n+1(CH
3)
3nBr (n=12,14,16,18) mixes with the molar ratio of distilled water according to 1:800, is stirred to dissolving;
In solution, pipette tetraethoxy, the molar ratio of tetraethoxy and quaternary surfactant is 1:(0.1 ~ 0.3);
Add pH to 8 ~ 11 of ammoniacal liquor regulator solution, be stirred to and produce white chunks gel;
Filtration, washing, drying, calcine the white powder of gained, obtain dual model mesoporous silicon oxide nanomaterial at temperature 550 DEG C.
4. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, it is characterized in that, in described step one, pretreated method is: dual model mesoporous silicon oxide nanomaterial was 120 DEG C, vacuum activation 3 hours.
5. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, it is characterized in that, described organic fluorescence molecule is the one in dipyridyl derivatives class, and the molecular structure of dipyridyl derivatives is:
Wherein R represents H, L-PROLINE, N-carbobenzoxy-(Cbz)-prolineamide, 3-CH
3c
6h
4cO, (CH
3)
3cO or CH
3cO.
6. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, it is characterized in that, the mass ratio of described organic fluorescence molecule and dual model mesoporous silicon oxide nanomaterial is (0.1-30): 100.
7. the preparation method of hybrid inorganic-organic fluorescent mesoporous silicon oxide nanomaterial as claimed in claim 1, it is characterized in that, the temperature that in described step 2, dual model mesoporous silicon oxide nanomaterial and the dichloromethane solution containing organic fluorescence molecule react is 40 ~ 45 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121589A (en) * | 2021-04-23 | 2021-07-16 | 吉林大学 | 1, 8-naphthalimide-based organic material, organic-inorganic hybrid nano material, preparation method and application |
| CN113502153A (en) * | 2021-07-07 | 2021-10-15 | 哈尔滨工程大学 | Non-aromatic luminous micromolecule/SiO2Hybrid fluorescent nano material and preparation method and application thereof |
| CN113717548A (en) * | 2020-05-25 | 2021-11-30 | 中国石油化工股份有限公司 | Surface-modified silica gel and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100272957A1 (en) * | 2003-03-27 | 2010-10-28 | Nippon Steel Corporation | Inorganic--organic hybrid-film-coated stainless-steel foil |
| CN103194210A (en) * | 2013-04-15 | 2013-07-10 | 北京工业大学 | Preparation method for SiO2-based organic-inorganic hybridized fluorescent material |
| CN104014251A (en) * | 2014-06-05 | 2014-09-03 | 北京工业大学 | Preparation method for inorganic particle hybrid polyelectrolyte nano-filtration membrane assembled based on inorganic supporting body |
-
2015
- 2015-12-01 CN CN201510863235.8A patent/CN105315990B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100272957A1 (en) * | 2003-03-27 | 2010-10-28 | Nippon Steel Corporation | Inorganic--organic hybrid-film-coated stainless-steel foil |
| CN103194210A (en) * | 2013-04-15 | 2013-07-10 | 北京工业大学 | Preparation method for SiO2-based organic-inorganic hybridized fluorescent material |
| CN104014251A (en) * | 2014-06-05 | 2014-09-03 | 北京工业大学 | Preparation method for inorganic particle hybrid polyelectrolyte nano-filtration membrane assembled based on inorganic supporting body |
Non-Patent Citations (3)
| Title |
|---|
| 孙继红等: "介孔SiO2负载1，8-萘二酸酐结构表征及其荧光性能", 《北京工业大学学报》 * |
| 王金鹏: "有机-无机致密纳米SiO2杂化荧光材料的制备与发光性能研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
| 高琳等: "双模型介孔SiO2二次孔结构对布洛芬装载和释放性能的影响", 《无机材料学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113717548A (en) * | 2020-05-25 | 2021-11-30 | 中国石油化工股份有限公司 | Surface-modified silica gel and preparation method and application thereof |
| CN113121589A (en) * | 2021-04-23 | 2021-07-16 | 吉林大学 | 1, 8-naphthalimide-based organic material, organic-inorganic hybrid nano material, preparation method and application |
| CN113121589B (en) * | 2021-04-23 | 2022-03-11 | 吉林大学 | 1, 8-naphthalimide-based organic material, organic-inorganic hybrid nano material, preparation method and application |
| CN113502153A (en) * | 2021-07-07 | 2021-10-15 | 哈尔滨工程大学 | Non-aromatic luminous micromolecule/SiO2Hybrid fluorescent nano material and preparation method and application thereof |
| CN113502153B (en) * | 2021-07-07 | 2023-02-14 | 哈尔滨工程大学 | Non-aromatic luminous micromolecule/SiO 2 Hybrid fluorescent nano material and preparation method and application thereof |
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