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Preparation method and application of tar-based carbon quantum dots

A tar-based carbon and quantum dot technology, applied in chemical instruments and methods, measuring devices, nanotechnology, etc., can solve problems such as high requirements and inability to detect quickly, and achieve high sensitivity, meet the requirements of offshore operations, and take up less land. Effect

Inactive Publication Date: 2019-03-26
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although this detection method is simple to operate and low in cost, it still needs to add a masking agent to pretreat the water sample, which requires high requirements and can only be carried out within a specific range, so it cannot be detected quickly

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  • Preparation method and application of tar-based carbon quantum dots
  • Preparation method and application of tar-based carbon quantum dots
  • Preparation method and application of tar-based carbon quantum dots

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preparation example Construction

[0044] The invention provides a preparation method and application of tar-based carbon quantum dots, such as figure 2 shown.

[0045] The preparation method comprises steps as follows:

[0046] (1) The biomass tar is rotatably distilled at 100°C-200°C, the fractions are collected, and prepared into an aqueous solution of biomass tar with a mass fraction of 10%-30%, and a certain volume of nitrogen-containing small molecules with a concentration of 0.1-1g / mL is added solution, mix well;

[0047] (2) Transfer the homogeneously mixed solution in step (1) to a reaction kettle with a polytetrafluoroethylene liner. After ultrasonic treatment in a mechanical ultrasonic cleaner for 5 to 15 minutes, put it into a muffle furnace and heat it at 160°C to 220°C. Keep warm at ℃ for 0.5h~2h, then cool down to room temperature naturally;

[0048] (3) Filter the solution obtained in step (2) with a 0.22 μm microporous membrane, then dialyze in a dialysis bag with a molecular weight of 3500...

Embodiment 1

[0066] The biomass tar was rotary distilled at 150°C, the fractions were collected, and configured into a tar aqueous solution with a mass fraction of 15%. Take 10mL of the above tar aqueous solution and 1mL of a concentration of 0.5g / mL polyethyleneimine solution, mix well, and transfer to 50mL polytetrafluoroethylene Put it in an ethylene reaction kettle, put it in a muffle furnace, keep it at 180°C for 1.5h, take it out, and cool it to room temperature. Filter the obtained brown-yellow solution with a 0.22 μm microporous membrane, and then dialyze it in a dialysis bag with a molecular weight of 3500 Da for 24 hours. The yield reached 27.6%.

[0067] image 3 For adding Cu 2+ Before and after different metal ions on the above PEI-CQDs fluorescence intensity diagram, in the presence of different metal ions, adding the same amount of Cu 2+ (white), F / F 0 The values ​​are all decreased, indicating that the addition of Cu 2+ Afterwards, PEI-CQDs all had a strong quenching e...

Embodiment 2

[0071] The biomass tar was rotatively distilled at 180°C, the fractions were collected, and configured into a tar aqueous solution with a mass fraction of 10%. Take 10mL of the above tar aqueous solution and 1.5mL of a concentration of 0.3g / mL ethylenediamine solution, mix well, and transfer to 50mL polytetrafluoroethylene Put it in an ethylene reactor, put it in a muffle furnace, keep it at 200°C for 1 hour, take it out, and cool it to room temperature. The obtained brown-yellow solution was filtered with a 0.22 μm microporous membrane, and then dialyzed in a dialysis bag with a molecular weight of 3500 Da for 24 h, and the dialysate was vacuum-dried at 80° C. for 1.5 h to obtain reddish-brown tar-based carbon quantum dots (N-CQDs), which The fluorescence yield is up to 31.4%.

[0072] Figure 6 It is the fluorescence quenching effect of different metal ions on N-CQDs (black), it can be seen that only Fe 3+ Can significantly quench the fluorescence intensity of N-CQDs, F / F ...

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Abstract

The invention provides a preparation method and application of tar-based carbon quantum dots, particularly relates to application of the tar-based carbon quantum dots to rapid evaluation of metal ionsin leaching liquid systems of deep-sea mineral resources, namely ocean manganese nodules and cobalt-rich crusts, and belongs to the field of carbon nanomaterial preparation technologies and application. According to the preparation method, the tar-based carbon quantum dots are firstly prepared. The tar-based carbon quantum dots serve as a fluorescent probe and have a selective fluorescence quenching effect with copper and iron ions in polymetallic and high-concentration ion leaching liquid of the oceanic manganese nodules and the cobalt-rich crusts under ultraviolet light stimulation, and thelinear relationship between the concentrations of Cu2+ and Fe3+ and fluorescence quenching can be obtained without pretreatment of the leaching liquid, so that the concentrations of Cu2+ and Fe3+ arecalculated. According to the method, leaching of copper, manganese, cobalt, nickel and iron in the high-concentration and polymetallic leaching system of the oceanic manganese nodules and the cobalt-rich crusts can be quickly evaluated, the capability of resisting to non-target detection ion interference is high, selectivity and sensitive are high, the detection concentration is wide, the cost islow, environmental protection is achieved, a process is simple, and operation is convenient and fast.

Description

technical field [0001] The invention relates to the technical field of carbon nanomaterial preparation, in particular to a preparation method and application of tar-based carbon quantum dots, specifically the application in rapid evaluation of metal ions in the leach solution system of oceanic manganese nodules and cobalt-rich crusts in deep sea mineral resources. Background technique [0002] With the depletion of conventional mineral resources in the world, human beings gradually shift the development of mineral resources to the depths of the ocean. Oceanic manganese nodules and cobalt-rich crusts in deep-sea mineral resources are rich in copper, cobalt, nickel, platinum, manganese, iron, etc. A complex symbiotic polymetallic mineral of valuable elements, containing more than 80 kinds of metal elements, among which the valuable metals copper, cobalt, nickel, and platinum mostly exist in MnO in the form of isomorphism 2 In the lattice, it is the most valuable marine mineral...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65B82Y20/00B82Y40/00G01N21/64
CPCB82Y20/00B82Y40/00C09K11/65G01N21/643G01N2021/6432
Inventor 冯雅丽边振忠李浩然邓祥意
Owner UNIV OF SCI & TECH BEIJING
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