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Carbon quantum dot fluorescent labeling material using coke powder as carbon source and preparation method thereof

A carbon quantum dot and fluorescent labeling technology, which is applied in the field of carbon quantum dot fluorescent labeling materials and their preparation, can solve the problems of low fluorescence yield of carbon quantum dots, harsh preparation conditions, difficult separation and purification, etc., and achieves easy emission and optical performance. Good, low cost effect

Active Publication Date: 2018-09-07
武汉科技大学资产经营有限公司
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Problems solved by technology

[0003] At present, the preparation methods of fluorescent carbon quantum dots are mainly summarized as top-down and bottom-up synthesis methods: top-down preparation methods often require relatively harsh reaction conditions, strict experimental conditions and high cost, and are not widely applicable. Poor, and the fluorescence yield of the prepared carbon quantum dots is low; while the bottom-up preparation method is to directly synthesize fluorescent carbon quantum dots by pyrolysis or carbonization of suitable precursors, the cost is high, and the fluorescence yield of carbon quantum dots is relatively high. low yield and difficult to separate and purify
[0004] Zhu H et al. (Zhu H, Wang X L, Li Y L, et al. Microwave synthesis fluorescent carbon nanoparticles with electrochemiluminescence properties[J]. Chem. Commun., 2009, 14 (34):5118-5120) combined PEG200 and carbohydrates The aqueous solution was subjected to microwave heating treatment to prepare C-QDs, and by changing the time of microwave treatment, carbon quantum dots with different fluorescence properties were obtained. The fluorescence quantum yield was only 3.1%~6.3%, and it was not easy to separate and purify.
[0005] "A preparation method of fluorescent carbon quantum dot probe for detecting beryllium in water" (CN 104003370 A) patent technology, the specific steps of this technology are to react the mixture of urea and citric acid at 200~240℃ for 5~7h Obtain a brown aqueous solution, and then obtain the product after the brown aqueous solution is subjected to centrifugal dialysis, rotary evaporation, and vacuum drying. The preparation conditions of this technology are harsh, the operation is complicated, and the promotion is relatively poor.

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  • Carbon quantum dot fluorescent labeling material using coke powder as carbon source and preparation method thereof
  • Carbon quantum dot fluorescent labeling material using coke powder as carbon source and preparation method thereof
  • Carbon quantum dot fluorescent labeling material using coke powder as carbon source and preparation method thereof

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Embodiment 1

[0041] A carbon quantum dot fluorescent labeling material using coke powder as a carbon source and a preparation method thereof. The concrete steps of the method described in this embodiment are:

[0042] (1) Pressed coke powder: Concentrated H 2 SO 4 : Concentrated HNO 3 The mass ratio is 0.1:(11~13):(2~4), the coke powder is placed in the reaction kettle first, and then concentrated H 2 SO 4 and concentrated HNO 3 mixed acids to obtain a black mixture.

[0043] (2) Stir the black mixture at 95-105° C. for 11-12 hours, cool naturally, and separate the solid and liquid; add NaOH solution to the separated liquid to adjust the pH value to 7-9 to obtain a brown-black liquid.

[0044] (3) According to the volume ratio of brown-black liquid: acetone: isopropanol is 1: (1~1.5): (1.3~1.8), add acetone and isopropanol to the brown-black liquid, stir for 10~20min, Centrifuge at 6000~9000r / min for 30~40min, remove the supernatant, and obtain the lower layer solution.

[0045] (4...

Embodiment 2

[0048] A carbon quantum dot fluorescent labeling material using coke powder as a carbon source and a preparation method thereof. The concrete steps of the method described in this embodiment are:

[0049] (1) Pressed coke powder: Concentrated H 2 SO 4 : Concentrated HNO 3 The mass ratio is 0.1:(9~11):(3~4), the coke powder is placed in the reaction kettle first, and then concentrated H 2 SO 4 and concentrated HNO 3 mixed acids to obtain a black mixture.

[0050] (2) Stir the black mixture at 95-105° C. for 10-11 hours, cool naturally, and separate the solid and liquid; add NaOH solution to the separated liquid to adjust the pH value to 7-9 to obtain a brown-black liquid.

[0051] (3) According to the volume ratio of brown-black liquid: acetone: isopropanol is 1: (1~1.5): (1.5~2), add acetone and isopropanol to the brown-black liquid, stir for 10~20min, Centrifuge at 6000~9000r / min for 40~50min, remove the supernatant, and obtain the lower layer solution.

[0052] (4) A...

Embodiment 3

[0055] A carbon quantum dot fluorescent labeling material using coke powder as a carbon source and a preparation method thereof. The concrete steps of the method described in this embodiment are:

[0056] (1) Pressed coke powder: Concentrated H 2 SO 4 : Concentrated HNO 3 The mass ratio is 0.1:(13~15):(4~5), put the coke powder in the reaction kettle first, then add concentrated H 2 SO 4 and concentrated HNO 3 mixed acids to obtain a black mixture.

[0057] (2) Stir the black mixture at 95-105° C. for 8-10 hours, cool naturally, and separate the solid and liquid; add NaOH solution to the separated liquid to adjust the pH value to 7-9 to obtain a brown-black liquid.

[0058] (3) According to the volume ratio of brown-black liquid: acetone: isopropanol is 1: (1~1.5): (1~1.5), add acetone and isopropanol to the brown-black liquid, stir for 10~20min, Centrifuge at 6000~9000r / min for 50~60min, remove the supernatant, and obtain the lower layer solution.

[0059] (4) Accordi...

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Abstract

The invention relates to a carbon quantum dot fluorescent-labeled material with coke powder serving as a carbon source and a preparation method of the carbon quantum dot fluorescent-labeled material. According to the technical scheme, the mass ratio of the coke powder to concentrated H2SO4 to concentrated HNO3 is 0.1: (9-15):(3-5), firstly, the coke powder is put in a reaction kettle, then mixed acid of concentrated H2SO4 and concentrated HNO3 is added, the mixture is stirred for 8-12 hours at a temperature of 85-105 DEG C, and cooling and solid-liquid separation are performed; the pH value is regulated to 7-11, and a brown black liquid is obtained; the brown black liquid, acetone and isopropanol are stirred and centrifugalized, and a lower-layer solution is obtained; the brown black liquid and absolute ethyl alcohol are stirred and centrifugalized, and a carbon quantum dot solution is obtained; the carbon quantum dot solution is dried, and the carbon quantum dot fluorescent-labeled material with the coke powder serving as the carbon source is obtained. The carbon quantum dot fluorescent-labeled material with the coke powder serving as the carbon source has the characteristics that the reaction temperature is low, the process is simple, the cost is low, separation and purification are facilitated, the yield of carbon quantum dots is high, and industrialization is facilitated; the prepared carbon quantum dot fluorescent-labeled material with the coke powder serving as the carbon source has good optical performance and low cytotoxicity.

Description

technical field [0001] The invention belongs to a carbon quantum dot fluorescent marking material. In particular, it relates to a carbon quantum dot fluorescent marking material using coke powder as a carbon source and a preparation method thereof. Background technique [0002] In 2004, American scientists Scrivens and others discovered and isolated carbon quantum dots for the first time when purifying single-walled carbon nanotubes. Compared with traditional semiconductor metal quantum dots, the discovery of carbon quantum dots is very eye-catching. Because traditional quantum dots usually contain heavy metal ions, their toxicity is relatively high, which limits their application in the field of biomarkers. Carbon quantum dots are based on carbon elements, which are more biologically safe than previous fluorescent materials, and have little interference with the activity of biomolecules. Moreover, in the process of preparing carbon quantum dots, its surface contains a lar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/65B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/65
Inventor 丁玲周尽晖彭泽泽沈韦舟雷付煜曾艳赵希然
Owner 武汉科技大学资产经营有限公司
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