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Preparation method for organic phase carbon dots

An organic phase, carbon dot technology, applied in chemical instruments and methods, nanotechnology, nano-optics, etc., can solve the problems of complex sample separation, long experiment time, limited, etc., and achieve simple and fast process methods, simple and environmentally friendly reaction conditions. , the effect of reducing the reaction time

Active Publication Date: 2015-04-22
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there have been many reports on the use of quantum dots and carbon dots, but the research on aqueous phase carbon dots is the most, and there are not many reports on organic phase carbon dots, which greatly limits the use of carbon dots in organic catalysis, polymer composites, etc. Aspects of application
Although some people (201410046953.7; 201310740394.X) have studied carbon dots in organic solvent systems such as n-hexane and cyclohexane, they mainly use n-hexane and cyclohexane as solvents to study the formation of carbon dots by solutes in the solution. There are few reports on the preparation of pure solvent carbon dots
Liu et al. (LIU S, WANG L, TIAN J, et al. Acid-driven, microwave-assisted production of photoluminescent carbon nitride dots from N,N-dimethylformamide [J]. RSC Advances, 2011, 1(6): 951 ) reported using sulfuric acid and phosphoric acid as catalysts to prepare hydrophilic DMF carbon dots, but the separation of samples obtained by this method is more complicated, and the reaction system is an aqueous phase, which is not conducive to the experiment of organic phase
Jiang et al. (201410000767.4) reported the use of solvent reflux method and microwave method to prepare organic phase carbon dots, but limited by the experimental conditions, the experiment time must be long and the yield is not high

Method used

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  • Preparation method for organic phase carbon dots

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Take 20mL of N,N-dimethylformamide (DMF), put it into a hydrothermal reaction kettle, and heat the solvent for 12 hours at 300°C to obtain a carbon dot solution. Filter the obtained liquid with a 0.2 μm microporous membrane, collect the distilled solvent DMF through rotary distillation, and dry it in a vacuum oven to obtain carbon dot solids (named DMF-CDs). Put the separated DMF into the hydrothermal reactor, and continue the reaction under the same conditions to obtain DMF-CDs. To detect carbon dots, such as Figure 1-5 As shown, among them, figure 1 It is the infrared spectrum of DMF-CDs carbon dots. It can be seen from the figure that there is a strong peak at around 1700, indicating that there are carbonyl groups in the carbon dots; figure 2 It is the transmission electron micrograph and particle size distribution diagram of DMF-CDs carbon dots. It can be seen from the figure that the size distribution of carbon dots is 2-4 nm, with an average size of about 3 nm...

Embodiment 2

[0030] Take 20mL of n-hexane (H), put it into the autoclave, and heat the solvent for 10h at 150°C to obtain the carbon dot solution. Filter the obtained liquid with a 0.2 μm microporous membrane, collect the distilled solvent through rotary distillation, and dry it in a vacuum oven to obtain n-hexane carbon dot solids (H-CDs). Put the separated n-hexane into the high-pressure reactor, continue the reaction under the same conditions, and continue to obtain H-CDs. The normal hexane obtained by the rotary steaming of the raw material n-hexane and the product is determined by gas chromatography, and the spectra are compared, as shown in Image 6 shown, from Image 6 It can be seen that there is no significant difference between the two spectra. Therefore, the separated solvent can also continue to react.

Embodiment 3

[0032] Take 20mL of N,N-dimethylacetamide (DMAc), put it into the autoclave, and heat the solvent at 200°C for 24 hours to obtain the carbon dot solution. The obtained liquid was filtered with a 0.2 μm microporous membrane, and the obtained liquid was collected by rotary distillation to collect the evaporated solvent, and then dried in a vacuum oven to obtain DMAc carbon dot solids (named DMAc-CDs). Put the separated DMAc into the autoclave and continue the reaction under the same conditions to obtain DMAc-CDs. To detect carbon dots, such as Figure 7 Shown, TEM image and particle size distribution of DMAc carbon dots. It can be seen from the figure that the size of DMAc carbon dots is uniform, and the average size is about 3 nm.

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Abstract

The invention discloses a preparation method for organic phase carbon dots. The preparation method comprises the steps that raw material are fetched and added into a reaction kettle, and the raw materials are subjected to a solvothermal reaction for 0.5-72 hours under the condition of 150-300 DEG C, so that an organic phase carbon dot solution is obtained; liquid is concentrated, an obtained solvent returns to the reaction kettle for cycle use, and solid is dried to obtain organic phase carbon quantum dots, wherein the raw materials are one of or the composition of several of N,N-dimethyl formamide, N,N-dimethylacetamide, dimethyl sulfoxide, normal hexane, cyclohexane, methylbenzene and xylene. The technological method is simple and rapid, reaction conditions are simple and friendly to environment, yield is high, and reaction time is reduced. The adopted raw materials are cheap and easy to obtain, catalyst does not need to be added, and the solvent can continue to be recycled. The prepared organic phase carbon dots have good dispersity in an organic solvent, and have wide application in the fields of organic coating, substance detection, catalysis, fluorescent ink, novel nanocomposite, novel electrochemical electrodes, novel optical materials and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of quantum dots, and in particular relates to a preparation method of organic phase carbon dots. Background technique [0002] Quantum dots refer to nanoparticles with three-dimensional dimensions below 100nm. They are quasi-zero-dimensional materials, mainly composed of II-VI elements. Due to its specific structure, it has size quantum effect and dielectric confinement effect, and has luminescent properties, which can emit fluorescence. [0003] Quantum dots have many unique optical properties. Due to the unique properties of quantum dots, its excitation wavelength range is very wide; in addition, by controlling the size of the synthesized particles, quantum dots of different colors can be obtained; quantum dots have good stability and can be stored for a long time; Unique optical properties, it has a very wide range of applications in electronic devices, biological analysis, optica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65C01B31/02B82Y40/00B82Y20/00
Inventor 袭锴胡栋华顾江江邓国庆张秋红孟震
Owner NANJING UNIV
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