Preparation method of N-doped carbon quantum dots

A technology of carbon quantum dots and nitrogen doping, applied in chemical instruments and methods, nano-carbon, nanotechnology for materials and surface science, etc., can solve the complex preparation process and low quantum yield of carbon-based quantum dot materials and other issues, to achieve the effect of reducing production costs, low cost, and stable chemical properties

Inactive Publication Date: 2017-06-06
TCL CORPORATION
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing nitrogen-doped carbon quantum dots, which aims to solve the problems of

Method used

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preparation example Construction

[0015] The embodiment of the present invention provides a method for preparing nitrogen-doped carbon quantum dots, which includes the following steps:

[0016] S01. After mixing lignin and deionized water, adjust the pH of the system to be alkaline, and heat and stir for the first time to obtain a lignin dispersion; add carboxylation reagent and activator to the lignin dispersion, and stir at constant temperature After the reaction, centrifugal treatment is completed, the slurry-like product is collected, and carboxylated lignin is obtained after drying;

[0017] S02. After mixing the carboxylated lignin and deionized water, heat and stir for the second time to obtain a carboxylated lignin dispersion; add an amination reagent to the carboxylated lignin dispersion, and react with constant temperature stirring, Obtain an aminated lignin dispersion;

[0018] S03. Transfer the aminated lignin dispersion to an autoclave, and take it out after a constant temperature hydrothermal reaction ...

Embodiment 1

[0039] A method for preparing nitrogen-doped carbon quantum dots includes the following steps:

[0040] S11. Carboxylation of Lignin

[0041] 10g of lignin and 50g of deionized water were added to a 200mL three-necked flask, heated to 80℃ in a water bath, stirred at 800rpm and adjusted to pH=10, stirred at a constant temperature for 30min to obtain a lignin dispersion; then, 3g sodium perchlorate, 10g Dichloroacetic acid was sequentially added to the three-necked flask, stirring continued and reacted at a constant temperature for 3 hours. After the reaction, the reaction solution was transferred to a centrifuge tube, and centrifuged at 8000 rpm for 5 minutes, and centrifuged 3 times; finally, the muddy lignin at the bottom of the centrifuge tube was transferred to a vacuum drying oven and dried to obtain carboxylated lignin .

[0042] S12. Carboxylated lignin amination

[0043] 10g of carboxylated lignin and 50g of deionized water were added to a 200mL three-necked flask, stirred an...

Embodiment 2

[0047] A method for preparing nitrogen-doped carbon quantum dots includes the following steps:

[0048] S21. Lignin carboxylation

[0049] 10g of lignin and 50g of deionized water were added to a 200mL three-necked flask, heated in a water bath to 80℃, stirred at 800rpm and adjusted to pH=10, stirred at a constant temperature for 30min to obtain a lignin dispersion; then, 3g sodium perchlorate, 10g two Chloroacetic acid was sequentially added to the three-necked flask, stirring continued and reacted at constant temperature for 3h. After the reaction, the reaction solution was transferred to a centrifuge tube, and centrifuged at 8000 rpm for 5 minutes, and centrifuged 3 times; finally, the muddy lignin at the bottom of the centrifuge tube was transferred to a vacuum drying oven and dried to obtain carboxylated lignin .

[0050] S22. Carboxylated lignin amination

[0051] 10g of carboxylated lignin and 50g of deionized water were added to a 200mL three-necked flask, stirred and heated...

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Abstract

The invention provides a preparation method of N-doped carbon quantum dots. The preparation method comprises the steps of mixing lignin and deionzed water, adjusting pH of a system to be alkaline, heating and stirring for the first time to obtain lignin dispersion liquid; adding a carboxylation agent and an activating agent into the lignin dispersion liquid, stirring and reacting at constant temperature, after the completion of the reaction, performing centrifugal treatment, collecting a slurry state product, and drying to obtain carboxylated lignin; mixing the carboxylated lignin and deionzed water, heating and stirring for the second time to obtain carboxylated lignin dispersion liquid; adding an amination agent into the carboxylated lignin dispersion liquid, and stirring and reacting at constant temperature to obtain aminated lignin dispersion liquid; transferring the aminated lignin dispersion liquid into a high pressure reactor, performing constant-temperature hydrothermal reaction at 120 to 200 DEG C for 3 to 5h, then taking out, and placing reaction liquid into a mixture of ice and water to cool to room temperature; performing centrifugal treatment, dialysis and drying in sequence to obtain the N-doped carbon quantum dots.

Description

Technical field [0001] The invention belongs to the technical field of quantum dot synthesis, and in particular relates to a method for preparing nitrogen-doped carbon quantum dots. Background technique [0002] Due to its unique optical properties, quantum dot materials have been widely used in the fields of optoelectronic display, medical monitoring, and biosensors, and have become a research hotspot. However, on the one hand, traditional quantum dot materials contain heavy metal elements such as Cd and Te, which are not only costly, but also have strong biological toxicity; on the other hand, traditional quantum dot materials need to strictly control the water content of the system during the preparation process And oxygen content, which puts strict requirements on the synthesis equipment and technology of quantum dot materials. The above two shortcomings of traditional quantum dot materials limit the application and development of quantum dot materials. [0003] In recent yea...

Claims

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Application Information

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IPC IPC(8): C09K11/65C01B32/15B82Y30/00B82Y20/00
Inventor 丘洁龙
Owner TCL CORPORATION
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