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Preparation method of core-shell graphene quantum dot @ mesoporous silica nano-material

A technology of graphene quantum dots and mesoporous silica, which is applied in the field of nano-fluorescent materials, can solve the problems of small size and unfavorable application of GQDs, and achieve the effects of rich surface groups, excellent fluorescent properties, and efficient drug loading capacity

Active Publication Date: 2018-01-05
XUZHOU MEDICAL UNIV
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Problems solved by technology

However, the fluorescence emission wavelength of GQDs prepared by the above-mentioned Top-down and Bottom-up methods is mostly less than 500nm, located in the blue light region, and the shorter emission wavelength is not conducive to further application in vivo
Although it has been reported in the literature that GQDs emitting near-infrared fluorescence can be prepared by solution chemistry, which broadens its application in the field of medical imaging, the appropriate nanometer size is the primary consideration for nanomaterials used in vivo, and GQDs have a small Small size (less than 10nm), easily excreted through the kidneys in the body, which is not conducive to playing a role in medical imaging or nano drug delivery systems

Method used

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  • Preparation method of core-shell graphene quantum dot @ mesoporous silica nano-material
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  • Preparation method of core-shell graphene quantum dot @ mesoporous silica nano-material

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preparation example Construction

[0033] Preparation method of core-shell GQDs@hMSN:

[0034] (1) Weigh 4-bromobenzyl bromide and N,N-dimethyldodecylamine (molar ratio 1:1.3) and dissolve in dichloromethane-methanol solution (V:V=3:2) , stirred at room temperature for 12 h under a nitrogen atmosphere, the reaction solution was concentrated by distillation under reduced pressure, the concentrated solution was transferred to diethyl ether to disperse, and left to stand until the precipitate was completely separated out. The precipitate was filtered and vacuum-dried to obtain a white crystalline solid, hereinafter referred to as "compound 1".

[0035] (2) Weigh compound 1,3-thiophene boronic acid, sodium carbonate and 4-(triphenylphosphine) palladium (Pd(PPh 3 ) 4 ) (molar ratio 1:4.7:0.17:0.86), dissolved in ethanol-water solution (V:V=2:1), heated to 90°C under nitrogen atmosphere, and refluxed for 6h. The reaction solution was distilled under reduced pressure to remove ethanol, the residue was extracted wit...

Embodiment 1-6

[0041] Examples 1-6 all adopt the above method to prepare GQDs@hMSN nanoparticles, the difference is that the fluorescence performance of GQDs is controlled by adjusting the temperature and reaction time of the high-pressure reactor in step (4); Add different amounts of TEOS to control the particle size of hMSN; adjust the different etching temperature and time used in step (6) to control the shell thickness of hMSN. The relevant experimental results are as follows:

[0042] The synthesis conditions of GQD quantum dots in each embodiment of table 1

[0043]

[0044]

[0045] GQDs products are generated from GQDs precursors in a high-pressure reactor. The higher the reaction temperature, the shorter the reaction time; the amount of TEOS added determines the diameter of the formed shell silica, and the greater the amount added, the final GQDs@hMSN particles will be generated The larger the diameter; the temperature and time for etching silicon dioxide with sodium carbonat...

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Abstract

The invention discloses a preparation method of core-shell graphene quantum dot @ mesoporous silica nano-material. The material employs graphene quantum dots as a core and hollow mesoporous silica asa shell, the diameter of nanometer particle is 80-120nm, and fluorescence emission wavelength is 570-670nm. The GQDs prepared by an organic synthesis method are used as a core, hMSN is used as a shellfor preparing GQDs@hMSN. The water soluble GQDs prepared by an organic phase synthesis method, GQDs is directly used as a core, in order to prepare the graphene quantum dot @ mesoporous silica nanometer particles, and after chemical etching, a compound with GQDs optical performance, a hMSN hollow meso-structure and abundant surface charges is prepared. The material has excellent optical properties and a hollow meso-structure, and the material can be applied to optical imaging and medical treatment in organism or diagnosis and treatment of tumor.

Description

technical field [0001] The invention belongs to the technical field of nano fluorescent materials, and in particular relates to a graphene quantum dot@mesoporous hollow silica (GQDs@hMSN) composite material and a preparation method thereof. Background technique [0002] Graphene Quantum Dots (GQDs) is a member of the carbon quantum dot family. It does not use any toxic metals (such as cadmium, lead, etc.) in its structure, and has good biocompatibility and excellent fluorescence properties. It has great application potential in medical diagnosis and treatment. The synthesis methods of graphene quantum dots mainly focus on Top-down and Bottom-up methods, in which the Top-down method is to break large-sized graphene into small-sized graphene quantum dots by physical or chemical methods, mainly including hydrothermal method , solvothermal method, strong acid oxidation method, and electrochemical method. Due to the randomness of the fragmentation point, the size and shape of GQ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65C09K11/02A61K47/04A61K47/52A61P35/00
Inventor 杨冬芝姚欣悦孙世安杜岩汤道权王娜董睛睛
Owner XUZHOU MEDICAL UNIV
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