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A kind of preparation method of core-shell graphene quantum dots@mesoporous silica nanomaterials

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

Active Publication Date: 2020-08-14
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 500 nm, which is 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 10 nm), 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 example Construction

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

[0034] (1) Weigh 4-bromobenzyl bromide and N, N-dimethyldodecylamine (1:1.3 molar ratio) and dissolve in dichloromethane-methanol solution (V:V =3:2) , stirred at room temperature under a nitrogen atmosphere for 12 h, the reaction solution was concentrated by vacuum distillation, 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 6 h. The reaction solution was distilled under reduced pressure to remove ethanol, the residue was extracted with an appro...

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); The particle size of hMSN is controlled by adding different amounts of TEOS; the shell thickness of hMSN is controlled by adjusting different etching temperatures and times used in step (6). The relevant experimental results are as follows:

[0042] Table 1 Synthesis conditions of GQD quantum dots in each embodiment

[0043]

[0044] 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 carbonate d...

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Abstract

The invention discloses a preparation method of core-shell graphene quantum dot@mesoporous silica nanomaterial, which is a core-shell nanoparticle with graphene quantum dot as the core and hollow mesoporous silica as the shell , the diameter of the nanoparticles is 80-120 nm, and the fluorescence emission wavelength is 570-670 nm. In this method, GQDs prepared by an organic synthesis method are used as the core, and hMSN is used as the shell to prepare GQDs@hMSN. This method uses the organic phase synthesis method to prepare water-soluble GQDs, and directly uses GQDs as the core to prepare graphene quantum dots@dense silica nanoparticles, and chemically etches to prepare GQDs with optical properties, hMSN hollow mesoporous structure and rich Complex surface charges. The material has excellent optical properties and a hollow mesoporous structure, and can be applied to in vivo optical imaging and medical treatment or diagnosis and treatment of tumors.

Description

technical field [0001] The invention belongs to the technical field of nano fluorescent materials, in particular 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 GQDs prepared ...

Claims

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Application Information

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Patent Type & Authority Patents(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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